Tag: M.W=300-400

Synthetic Route of 43204-63-3, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 43204-63-3 as follows.

EXAMPLE 1 A mixture of 5-aminooxindol (14 g), 29 g of bis(beta-bromoethyl)amine.hydrobromide in 250 ml of ethanol was stirred under reflux for 8 hours and allowed to stand overnight at room temperature. To the mixture was added sodium carbonate (10.1 g) and the mixture was stirred further for 8 hours under reflux. After cooling to room temperature, crystals which precipitated were collected by filtration and recrystallized from a mixture of water and ethanol to give 16 g of 5-(1-piperazinyl)oxindol.hydrobromide. Pale yellow powdery crystal NMR (200 MHz, DMSO-d6) delta: 3.30 (8H, s), 3.47 (2H, s), 6.78 (1H, d, J=8.5 Hz), 6.90 (1H, dd, J=8.5 Hz, 2 Hz), 7.04 (1H, d, J=2 Hz), 8.88 (2H, brs), 10.27 (1H, s)

According to the analysis of related databases, 43204-63-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Otsuka Pharmaceutical Co., Ltd.; US4737501; (1988); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 955959-84-9, Formula: C18H11BrO

In this example, a method for synthesizing N-(l, r-biphenyl-4-yl)-N-[4-(dibenzofuran-4-yl)phenyl]-9,9-dimethyl-9H-fluoren-2-ami ne (abbreviation: FrBBiF-II) represented by Structural Formula (100) will be described. [0238] [0239] First, 2.1 g (6.6 mmol) of 4-(4-bromophenyl)dibenzofuran, 2.4 g (6.7 mmol) of N-(l,l ‘-biphenyl-4-yl)-9,9-dimethyl-9H-fluoren-2-amine, and 1.9 g (20 mmol) of sodium tert-butoxide were put in a 200-mL three-neck flask and the air in the flask was replaced with nitrogen. To this mixture, 33 mL of toluene, 0.30 mL of a 10 % hexane solution of tri(ter/-butyl)phosphine, and 48 mg (0.1 mmol) of bis(dibenzylideneacetone)palladium(0) were added, and stirring was performed at 90 C for 7.5 hours. After the stirring, suction filtration through Florisil (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 540-00135), Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531 – 16855), and alumina was carried out to give a filtrate. The filtrate was concentrated to give a solid. The solid was purified by silica gel column chromatography (the developing solvent was hexane and toluene in a ratio of 3:1) to give a solid. The solid was recrystallized from toluene and hexane, so that 3.2 g of an objective solid was obtained in a yield of 81 %. A reaction scheme of this reaction is shown below. [0240] [0241] Using a train sublimation method, 1.0 g of the obtained solid was purified by sublimation. In the purification by sublimation, the pressure was 2.6 Pa, the flow rate of argon gas was 5.0 mL/min, and the temperature of the heating was 289 C. After the purification by sublimation, 0.99 g of a solid which was the object of the synthesis was obtained at a collection rate of 95 %. [0242] Results of measurement of the obtained solid by nuclear magnetic resonance ( NMR) are shown below. NMR (CDCI3, 500 MHz): delta = 1.46 (s, 6H), 7.18 (dd, J = 8.5 Hz, 2.5 Hz, 1 H), 7.26-7.48 (m, 14H), 7.53-7.56 (m, 2H), 7.60-7.68 (m, 6H), 7.86-7.91 (m, 3H), 7.99 (d, J = 7.5 Hz, 1 H). [0243] Thermogravimetry-differential thermal analysis (TG-DTA) of the obtained FrBBiF-II was performed. The measurement was conducted by using a high vacuum differential type differential thermal balance (TG/DTA 2410SA, manufactured by Bruker AXS Kappa.Kappa.)· The measurement was carried out under a nitrogen stream (a flow rate of 200 mL/min) and a normal pressure at a temperature rising rate of 10 C/min. The relationship between weight and temperature (thermogravimetry) shows that the 5 % weight loss temperature is 393 C, which is indicative of high heat resistance. [0244] FIGS. 13A and 13B are NMR charts. Note that FIG. 13B shows an enlarged part of FIG. 13A in the range of 7.00 ppm to 8.25 ppm. The measurement results confirmed that N-(l, -biphenyl-4-yl)-N-[4-(dibenzofuran-4-yl)phenyl]-9,9-dimethyl-9H-fluoren-2-ami ne (abbreviation: FrBBiF-II), which was the target substance, was obtained. [0245] Physical Properties of FrBBiF-Il FIG. 14A shows an absorption spectrum and an emission spectrum of FrBBiF-II in a toluene solution of FrBBiF-II, and FIG. 14B shows an absorption spectrum and an emission spectrum of a thin film of FrBBiF-II. The spectra were measured with a UV-visible spectrophotometer (V550, produced by JASCO Corporation). The spectra of FrBBiF-II in the toluene solution of FrBBiF-II were measured with a toluene solution of FrBBiF-II put in a quartz cell. The spectra of the thin film were measured with a sample prepared by deposition of FrBBiF-II on a quartz substrate by evaporation. Note that in the case of the absorption spectrum of FrBBiF-II in the toluene solution of FrBBiF-II, the absorption spectrum obtained by subtraction of the absorption spectra of the quartz cell and toluene from the measured spectra is shown in the drawing and that in the case of the absorption spectrum of the thin film of FrBBiF-II, the absorption spectrum obtained by subtraction of the absorption spectrum of the quartz substrate from the measured spectra is shown in the drawing. [0246] As shown in FIG. 14A, in the case of FrBBiF-II in the toluene solution, an absorption peak was observed at approximately 360 nm, and an emission wavelength peak was observed at approximately 415 nm (excitation wavelength: 366 nm). As shown in FIG. 14B, in the case of the thin film of FrBBiF-II, absorption peaks were observed at approximately 368 nm, 294 nm, 266 nm, 247 nm, and 209 nm, and an emission wavelength peak was observed at approximately 428 nm (excitation wavelength: 376 nm). Thus, it was found that absorption and light emission of FrBBiF-II occur in extremely short wavelength regions. [0247] The ionization potential of FrBBiF-II in a thin film state was measured by photoelectron spectroscopy (the measuring instrument: AC-2, manufactured by Riken Keiki, Co., Ltd.) in the air. The obtained value of the ionization potential was converted into a negative value, so that the HOMO level of FrBBiF-II was determined to be -5.61 eV. From the da…

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SEMICONDUCTOR ENERGY LABORATORY CO., LTD.; OGITA, Kaori; SEO, Satoshi; SEO, Hiromi; TAKAHASHI, Tatsuyoshi; WO2014/157018; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 955959-84-9, 955959-84-9

6.3 g (15.4 mmol) of N-phenyl-3,3-bicarbazole, 5.0 g (15.4 mmol) of 4-(4-bromophenyl)dibenzo[b,d]furan, 3.0 g (30.7 mmol) of sodium t-butoxide, 0.9 g (1.5 mmol) of tris(dibenzylideneacetone)dipalladium, and 1.2 mL of tri t-butylphosphine (50% in toluene) were mixed with 100 mL of xylene in a 250 mL round flask, and the mixture was heated and refluxed under a nitrogen flow for 15 hours. The obtained mixture was added to 300 mL of methanol, and a solid crystallized therein was filtered, dissolved in dichlorobenzene, filtered with silica gel/Celite, and after removing an appropriate amount of an organic solvent, recrystallized with methanol to obtain Compound B-78 (7.3 g, a yield of 73%). (0183) calcd. C48H30N2O: C, 88.59; H, 4.65; N, 4.30; O, 2.46. found: C, 88.56; H, 4.62; N, 4.20; 0, 2.43.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-(4-Bromophenyl)dibenzo[b,d]furan, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SAMSUNG SDI CO., LTD.; JUNG, Ho Kuk; LUI, Jinhyun; KIM, Dong-Yeong; JANG, Kipo; HUH, Dal-Ho; YU, Eun Sun; JUNG, Sung-Hyun; (75 pag.)US2019/280211; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 10016-52-1,Some common heterocyclic compound, 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, molecular formula is C12H6Br2O, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a two-necked flask were added A-1-1 (2.5 g), B-1 (3.6 g) And sodium tert-butoxide (4.4 g) was added thereto. The flask was filled with di-gassed toluene (46 mL) and heated to 100 C. Pd [P (t-Bu) 3] 2 (200 mg), Pd And the mixture was stirred at the same temperature for 17 hours. Diluted with DCM (100 mL) and filtered through SiO2. The filtered solution was depressurized to remove the solvent, and the residue was dissolved in THF in EA and then recrystallized to obtain A-1 (final) (1.5 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,8-Dibromodibenzo[b,d]furan, its application will become more common.

Reference:
Patent; LG Chem, Ltd.; Lee Chung-hwan; Bae Jae-sun; Lee Jae-cheol; Kim Hwa-gyeong; Shin Ji-yeon; (37 pag.)KR2018/92782; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 52997-43-0, name is 7-(Bromomethyl)pentadecane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 52997-43-0

General procedure: General procedure for the synthesis of a1-a6: To a solution of indoline-2,3-diones (10 mmol) in DMF (40 mL) was added K2CO3(15 mmol, 2.073 g) and 7-(bromomethyl)pentadecane (11 mmol,3.358 g) under nitrogen. The mixture was stirred at 70 C and monitoredby TLC. After the reaction completed, water was added, andextracted with EtOAc. The organic layer was combined and dried withMgSO4. After evaporation of the solvent, the residue was purified bycolumn chromatograph (eluent: Petroleum/EtOAc=20:1) to give thetarget compound.

The synthetic route of 7-(Bromomethyl)pentadecane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hu, Qian; Jiang, Hua; Cui, Zhihua; Chen, Weiguo; Dyes and Pigments; vol. 173; (2020);,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 201138-91-2,Some common heterocyclic compound, 201138-91-2, name is 4,6-Dibromodibenzo[b,d]furan, molecular formula is C12H6Br2O, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Under an argon atmosphere, to a 1,000 ml Erlenmeyer flask, 4,6-dibromodibenzofuran (16.3 g, 50 mmol), phenylboronic acid (6.71 g, 55 mmol), K2CO3 (20.7 g, 150 mmol), Pd(PPh3)4(2.89 g, 2.5 mmol), 500 ml of a mixture solution of toluene/EtOH/H2O (4/2/1) were added in order, followed by heating and refluxing at a temperature of about 80 C. for about 5 hours. Then, the reaction mixture was cooled to room temperature, and toluene was added thereto. An aqueous layer was removed, and an organic layer was washed with a saline solution and dried with MgSO4. MgSO4 was filtered and separated, and an organic layer was concentrated. The crude product thus obtained was separated by silica gel column chromatography (using a mixture solvent of hexane/toluene) and recrystallized to obtain Intermediate A as a white solid (12.1 g, yield 75%). The structure of the product was identified using FAB-MS (m/z=323).

The synthetic route of 201138-91-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Display Co., Ltd.; UNO, Takuya; (209 pag.)US2019/165285; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, A new synthetic method of this compound is introduced below., HPLC of Formula: C18H11BrO

Argon atmosphere, the compound (vii) in a 100mL three-necked flask 1.50g, Compound (xi) 0.87g, bis(dibenzylideneacetone)palladium (0) (Pd(dba)2) 0.11g, tri-t-butylphosphine ((t-Bu)3P) 0.15g, was added to sodium t-butoxide 0.54g, it was heated under reflux for 7 hours in 45mL of toluene solvent. After air-cooling, water was added The organic layer was separated, and the solvent was distilled off. The crude product thus obtained was purified by silica gel column chromatography (dichloro methane and using a mixed solvent of hexane), toluene, and subjected to recrystallization with hexane mixed solvent to give the compound A-41 as a white solid 1.86g (89percent yield).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Samsung DisplayCo., Ltd.; Huchiwaki, Junta; Oyama, Hiromi; Miyata, Yasuo; Sakamoto, Naoya; Ueno, Masatsuku; Takada, Echinori; (155 pag.)KR2015/90021; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 10016-52-1, A common heterocyclic compound, 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, molecular formula is C12H6Br2O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

[0001083] To a solution of Compound 302B (324 mg, 1 mmol) in THF (20 mL) was added n-BuLi (2.5 M, 0.4 mL, 1.06 mmol) under nitrogen at -60 C. It was stirred at -60 C for 0.5 h. And then a solution of diethyl oxalate (0.4 mL, 3 mmol) in THF (5 mL) was added. The mixture was stirred at -60 C for 0.5 h, quenched with saturated ammonium chloride solution (200 mL), extracted with ethyl acetate (20 mL x 3), washed with brine (20 mL), dried over anhydrous sodium sulfate, and purified with flash column chromatography on silica gel (ethyl acetate in petroleum ether, 5% v/v) to furnish Compound 302C.

The synthetic route of 10016-52-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHU, Daniel; BRIDGES, Alexander, James; WO2015/42397; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 72678-19-4, name is 2,6-Dibromo-4-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., Quality Control of 2,6-Dibromo-4-(trifluoromethyl)aniline

A mixture of 2,6-dibromo-4-trifluoromethylaniline (1.61 g, 5.04 mmol), acetic acid (4.8 ml) and propionic acid (2.4 ml) was cooled to an internal temperature of -5 C. or lower, and 40% nitrosylsulfuric acid (1.76 g, 5.54 mmol) was dropwise added thereto. After the addition and still at -5 C. or lower, this was stirred for 30 minutes to give a diazo liquid. In a separate vessel, a mixture of the intermediate A-3 (2.10 g, 5.04 mmol), tetrahydrofuran (10 mL), methanol (10 mL) and sulfamic acid (0.073 g, 0.76 mmol) was cooled to -5 C., and the diazo liquid was dropwise added thereto. This was stirred for 30 minutes still at -5 C., then restored to room temperature, and water was added thereto, and extracted with hexane. The hexane layer was dried with anhydrous sodium sulfate, concentrated under reduced pressure, and purified through silica gel column chromatography to give an intermediate C-3 (1.71 g, yield 46%) as an oily substance.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; MITSUBISHI CHEMICAL CORPORATION; SHIGA, Yasushi; AOBA, Mitsuya; TANAKA, Yuki; ISHIDA, Mio; US2015/191601; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 3975-77-7, name is 2-Bromo-1,3,5-tri-tert-butylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 2-Bromo-1,3,5-tri-tert-butylbenzene

A solution of bromo-2,4,6-tri-tert-butylbenzene (?supermesityl bromide, Mes*Br?, 326mg, 1.00mmol) in pentane (1.5mL) and THF (0.7mL) was cooled to-60C under argon gas cover for the injection of nBuLi (1.13mmol) in hexane (0.50mL). After one hour at rt, the supernatant was withdrawn from the precipitated 2,4,6-tri-tert-butylphenyllithium (Mes*Li), which was then washed with dry pentane (2×1mL). The subsequent addition of anhydrous Et2O (0.6mL) dissolved Mes*Li partially, and the entailing treatment with 2,2,6,6-tetramethylpiperidine (HTMP, 0.034mL, 28mg, 0.2mmol) consumed a corresponding portion of Mes*Li. The mixture was treated with the enone 10 (80mg, 0.30mmol) and kept at-60C for 1h, whereafter Mes*Li had been dissolved entirely. The solution was transferred to an NMR tube (5mm) and observed until 10 (deltaH=6.54ppm) had vanished (24h). The tube should be cooled in ice during the final addition of D2O (0.10mL). The resultant mixture was diluted with aqueous HCl (2M, 2mL) and Et2O (5mL). The acidic aqueous layer was shaken with Et2O (2×5mL) and discarded. The combined Et2O phases were washed with distilled water (3×3mL), dried over Na2SO4, filtered, and concentrated to leave a mixture (108mg) of 19, Mes*H, and partially (81%) deuteriated enone 10 in a 10:68:22M ratio. Analytically pure 19 had mp 202-203C (from 10mL of ethanol). (0032) IR (KBr) nu 3566 (very sharp O-H), 2961, 2870, 1595, 1485, 1474, 1458, 1362, 754cm-1. (0033) 1H NMR (CDCl3, 400MHz) delta 0.94 (s, 9H, 3×Me-1?), 1.04 (d, 4J=1.2Hz, 1H, OH), 1.25 (s, 3H, 5?-Mea), 1.31 (s, 18H, 2×meta-CMe3), 1.35 (s, 3H, 3-Mea), 1.40 (s, 3H, 3-Meb), 1.43 (s, 3H, 1-Mea), 1.49 (s, 3H, 1-Meb), 1.52 (s, 3H, 5?-Meb), 1.90 (d, 2J=15.2Hz, 1H, 4?-Ha), 2.70 (d, 2J=15.2Hz, 1H, 4?-Hb), 5.40 (d, 4J=1.2Hz, 1H, alpha-H), 7.12 (m, 1H, 4-H), 7.14 (m, 1H, 7-H), 7.18 and 7.19 (2m, 2H, 5-/6-H), 7.24 (d, 4J=1.7Hz, 2H, 2×ortho-H), 7.28ppm (t, 4J=1.7Hz, 1H, para-H), assigned through the NOESY correlations 3-Mea+b ? alpha-H ? 4?-Ha ? 4?-Hb ? ortho-H ? meta-C(CH3)3 ? para-H; 1-Mea ? 1-Meb ? HO ? ortho-H; 5?-Mea ? ortho-H ? 5?-Meb ? HO ? 1-Meb ? meta-C(CH3)3; (0034) 13C NMR (CDCl3, 100.6MHz) delta 26.3 (qsept, 1J=125.5Hz, 3J=4.9Hz, 3×Me-1?), 26.7 (qm, 1J=ca. 124 Hz, 5?-Meb), 31.2 (qm, 1J=124.5Hz, 1-Mea), 31.5 (qsept, 1J=125Hz, 3J=4.9Hz, 2×meta-CMe3), 32.30 and 32.32 (2 qm, 1J=126Hz, 1-Meb and 3-Meb), 33.2 (qm, 1J=126Hz, 3-Mea), 35.0 (quat, 2×meta-CMe3), 37.2 (qm, 1J=126.0Hz, 5?-Mea), 37.8 (quat, C-5?), 40.5 (quat, C-2?), 46.3 (quat, C-1), 48.7 (tm, 1J=124Hz, CH2-4?), 49.3 (quat, C-3), 81.3 (quat, C-3?), 120.0 (dt, 1J=153Hz, 3J=6.5Hz, C-para), 120.3 (dt, 1J=152Hz, 3J=6.5Hz, 2×C-ortho), 122.3 (dd, 1J=156Hz, C-7), 122.6 (dd, 1J=156Hz, C-4), 126.3 (dd, 1J=158Hz, 3J=7.4Hz, C-5), 126.8 (dd, 1J=158Hz, 3J=7.4Hz, C-6), 128.6 (dm, 1J=140.6Hz, C-alpha), 147.1 (quat, C-3a), 148.0 (quat, C-7a), 150.6 (sept, 3J=3.7Hz, 2×C-meta), 152.1 (quat, C-ipso), 154.1ppm (quat, C-2), assigned through the coupling constants, comparison with 13b, and the selective {1H} decoupling experiment {CH2 and all CH3} ? C-1 as a d with 3J=8Hz (trans to alpha-H), C-2 as a d with 2J=3.8Hz to alpha-H, C-ipso as a t with 3J=ca. 6 Hz, C-meta as a. Anal. calcd for C37H56O (516.9): C, 85.98; H, 10.92. Found: C, 85.93; H, 10.83.

The synthetic route of 3975-77-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Knorr, Rudolf; Schmidt, Barbara; Freudenreich, Johannes; von Roman, Therese; Tetrahedron; vol. 74; 52; (2018); p. 7466 – 7471;,
Bromide – Wikipedia,
bromide – Wiktionary