Tag: M.W=200-300

Related Products of 24358-62-1, A common heterocyclic compound, 24358-62-1, name is 1-(4-Bromophenyl)ethylamine, molecular formula is C8H10BrN, 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.

In addition to the foregoing, numerous other chromatographic separations using a column bonded with a CSP including a derivatized cyclofructan residue were carried out. Tables 5-9 list some additional examples of chromatographic separations using a column bonded with a CSP of the present invention. AU examples of chromatographic separations using columns bonded with CSPs of the present invention were carried out using the following experimental conditions and procedures.|0132| The high performance liquid chromatography (HPLC) column packing system was composed of an air driven fluid pump (HASKEL, DSTV- 122), an air compressor, a pressure regulator, a low pressure gauge, two high-pressure gauges (10,000 and 6,000 psi), a slurry chamber, check valves, and tubings. The CSPs were slurry packed into a 25 cm x 0.46 cm (inner diameter, I. D.) stainless steel column.|0133| The HPLC system was an Agilent 1 100 system (Agilent Technologies, Palo Alto,CA), which consisted of a diode array detector, an autosampler, a binary pump, a temperature- controlled column chamber, and Chemstation software. All chiral analytes were dissolved in ethanol, methanol, or other appropriate mobile phases, as indicated. For the LC analysis, the injection volume and flow rate were 5 muL and 1 mL/min, respectively. Separations were carried out at room temperature (~20 0C) if not specified otherwise. The wavelengths of UV detection were 195, 200, 210, and 254 nm. The mobile phase was degassed by ultrasonication under vacuum for 5 min. Each sample was analyzed in duplicate. Three operation modes (the normal phase mode, polar organic mode, and reversed phase mode) were tested, unless indicated otherwise. In the normal phase mode, heptane with ethanol or isopropanol was used as the mobile phase. In some cases, trifluoroacetic acid (TFA) was used as an additive, as indicated. The mobile phase of the polar organic mode was composed of acetonitrile/methanol and small amounts of acetic acid and triethylamine. Water/acetonitrile or acetonitrile/acetate buffer (20 mM, pH = 4.1 ) was used as the mobile phase in the reversed-phase mode.|0134| Two different supercritical fluid chromatographic instruments were used. One was a Berger SFC unit with an FCM 1200 flow control module, a TCM 2100 thermal column module, a dual pump control module, and a column selection valve. The flow rate was 4 mL/min. The cosolvent was composed of methanol/ethanol/isopropanol = 1 : 1 : 1 and 0.2% diethylamine (DEA). The gradient mobile phase composition was 5% cosolvent hold during 0- 0.6 min, 5-60% during 0.6-4.3 min, 60% hold during 4.3-6.3 min, 60%-5% during 6.3-6.9 min, and 5% hold during 6.9-8.0 min. The other SFC system was a Jasco (MD, USA) system comprised of an autosampler unit (AS-2059-SF Plus), a dual pump module (PU-2086 Plus), a column thermostat module (CO-2060 Plus), a UV/Vis detector (UV-2075 Plus), and a back pressure regulator module (SCH-Vch-BP). Unless otherwise specified, the mobile phase was composed of CCVmethanol (0.1 % TFA or 0.1% diethylamine). The flow rate was 3 mL/min.|0135| For the calculations of chromatographic data, the “dead time” to was determined by the peak of the refractive index change due to the sample solvent or determined by injecting l ,3,5-tri-/e/-/-butylbenzene in the normal phase mode.

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; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; ARMSTRONG, Daniel, W.; PING, Sun; BREITBACH, Zachary, S.; WANG, Chunlei; WO2010/148191; (2010); A2;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 118527-30-3, name is 2-Bromo-1,3-bis(trifluoromethyl)benzene, 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 118527-30-3, Application In Synthesis of 2-Bromo-1,3-bis(trifluoromethyl)benzene

General procedure: 12.6 g (38.32 mmol) of 9H-[3,9?]bicarbazolyl [18628-07-4], 7 g (38.32 mmol) of 2-bromo-1,3-ditrifluoromethylbenzene [118527-30-3] and 16 g of K2CO3are suspended in 300 mL of p-xylene. To the suspension are added 0.86 g (3.84 mmol) of Pd(OAc)2and 7.6 mL of a 1M tri-tert-butylphosphine solution. The reaction mixture is heated under reflux for 16 h. After cooling, the organic phase is removed, washed three times with 200 mL of water and then concentrated to dryness. The residue is subjected to hot extraction with toluene, recrystallized from toluene and finally sublimed under high vacuum. Yield: 14.5 g (35 mmol), 87% of theory; purity 99.9%

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; MerckPatent GMBH; Suttessel, Philip; Faram, AmirHossain; Blume, Christoph; Yatzi, Anya; (85 pag.)KR2015/132872; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 6274-57-3, A common heterocyclic compound, 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, molecular formula is C9H12BrN, 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.

General procedure: Pd(PPh3)4 (3 mol%) was added to a suspension of the appropriate benzoxazole 7 and (het)aryl bromide (1 equiv) in 1 M aq K2CO3 (3equiv) and 1,4-dioxane (0.15 M) at r.t. The mixture was stirred at reflux for 2 h then cooled to r.t. H2O was added, and the mixture was extracted with EtOAc. The organic layers were combined, washed with brine, dried (NaSO4), filtered, and concentrated in vacuo. The residue was purified by column chromatography (silica gel,hexane-EtOAc or CHCl3-MeOH).

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:
Article; Fukaya, Takayuki; Masumoto, Shuji; Synthesis; vol. 45; 23; (2013); p. 3269 – 3275;,
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. 40161-54-4, name is 1-Bromo-2-fluoro-4-(trifluoromethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H3BrF4

To a solution of 4-bromo-3-fluoro-benzotrifluoride (585 mg, 2.36 mmol) in 15 mL of THF, stirred at -75 C. under nitrogen atmosphere, 1.53 mL (2.6 mmol) of a 1.7M solution of tert-butyllithium in pentane were added dropwise. The reaction mixture was stirred at -60 C. for 15 minutes then a solution of 2-methyl-propane-2-sulfinic acid-(tetrahydro-pyran-4-ylidene)-amide (400 mg, 1.97 mmol; prepared as described in literature: WO2005/87751 A2) in 10 mL of THF was added dropwise. The reaction mixture was allowed to reach room temperature and stirred for 1 hr. A saturated ammonium chloride solution was added and the reaction mixtures was extracted with ethyl acetate. The organic phases were collected, dried over sodium sulfate and concentrated under vacuum. The crude obtained was purified by flash chromatography (eluent: cyclohexane/AcOEt; gradient from 12% to 100% of AcOEt). The oil obtained was diluted in 2 mL of 1,4-dioxane, 0.4 mL of a 4 M solution of hydrochloric acid in 1,4-dioxane were added, the reaction mixture was stirred at room temperature for 1 hr and then concentrated under vacuum to obtain 100 mg of the title compound as white solid.LC-MS (Method 2): Rt=0.90 minMS (ESI pos): m/z=264 (M+H)+

The synthetic route of 40161-54-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Boehringer Ingelheim International GmbH; HOENKE, Christoph; BERTANI, Barbara; FERRARA, Marco; FOSSATI, Giacomo; FRATTINI, Sara; GIOVANNINI, Riccardo; HOBSON, Scott; (88 pag.)US2017/101411; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

67567-26-4, name is 4-Bromo-2,6-difluoroaniline, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Application In Synthesis of 4-Bromo-2,6-difluoroaniline

Example 1 5-Bromo-1,3-difluoro-2-nitro-benzene: To a suspension of sodium perborate tetrahydrate (1.04 g, 5 mmol) in acetic acid (20 m]L), stirred at 55 C., was added a solution of 4-bromo-2,6-difluoroaniline in acetic acid (10 mL) over 1 hour in a dropwise fashion. After stirring at 55 C. for an additional 3 hours, the solution was allowed to cool to room temperature and filtered. The filtrate was poured into ice, and extracted twice with ethyl acetate. The combined organic extracts were washed successively with 5*100-mL portions of water, brine, dried (MgSO4), and concentrated in vacuo. The resulting residue was purified by column chromatography over silica gel eluted with ethyl acetate:hexanes (1:20) to afford 780 mg of the titel compound as a tan solid. 1H NMR (CDCl3) delta 7.32 (dt, 2H).

The synthetic route of 67567-26-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Charifson, Paul S.; Deininger, David D.; Grillot, Anne-Laure; Liao, Yusheng; Ronkin, Steven M.; Stamos, Dean; Perola, Emanuele; Wang, Tiansheng; LeTiran, Arnaud; Drumm, Joseph; US2005/256136; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 445303-69-5,Some common heterocyclic compound, 445303-69-5, name is 4-Bromo-2-(difluoromethyl)-1-fluorobenzene, molecular formula is C7H4BrF3, 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.

Preparation 4:4-[3-(DIFLUOROMETHYL)-4-FLUOROPHENYL]PYRIDINETo a mixture of 4-bromo-2-(diotafluoromethyl)-l-fluorobenzene (0.5 g, 2.24 mmol), 1- pyriotadyl-4-boroniotac acid (0.33 g, 2.69 mmol) and sodium carbonate (0.64 g, 5.6 mmol) in toluene/ethanol (1 : 1, 20 ml) under nitrogen, was added palladium tetrakis (0.13 g , 5 mol%). The mixture was heated at reflux for 16 h, cooled to ambient temperature and diluted with water (50 ml) and ethyl acetate (100 ml). The organic layer was separated and the aqueous phase was extracted with ethyl acetate (2×50 ml). The combined organic phases was evaporated to dryness and dissolved in aqueous hydrochloric acid (10%, 50 ml). The solution was washed with diethyl ether (2×40 ml), basified with aqueous sodium hydroxide (2M) and extracted with ethyl acetate (2×50 ml). The combined organic phases was dried (MgSO4) and evaporated to dryness to give the crude product. Purification by flash column chromatography (ethyl acetate/isooctane 2: 1) gave the title compound (0.34 g). MS m/z (rel. intensity, 70 eV) 223 (M+, bp), 222 (12), 204 (7), 172 (12), 145 (8).

The synthetic route of 445303-69-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; A. CARLSSON RESEARCH AB; WO2007/65655; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 626-40-4,Some common heterocyclic compound, 626-40-4, name is 3,5-Dibromoaniline, molecular formula is C6H5Br2N, 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.

Preparation of the compound 3-((3-cyano-6-cyclopropylpyridin-2-yl)thio)-N-(3,5-dibromophenyl)propanamide (19) I-3 (0.50) g, 2 mmol, 1 eq), EDCI (0.50 g, 2.6 mmol, 1.3 eq) and HOBT (0.08 g, 0.6 mmol, 0.3 eq) dissolved in DMF, not more than 10 C, The reaction was carried out for 30 min, and 3,5-dibromoaniline (0.56 g, 2.2 mmol, 1.1 eq) was added. the color of the reaction solution was darkened and reacted overnight at room temperature. The reaction was complete by TLC. Post-treatment: The reaction solution was poured into water, suction-filtered, and then filtered to give a crude product. The crude product was recrystallized from petroleum ether-ethyl acetate to afford LWTW-225 (150 mg, yield 31%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,5-Dibromoaniline, its application will become more common.

Reference:
Patent; Yao Da Pharmaceutical Co., Ltd.; Bian Jinlei; Zhao Lulu; Wang Jubo; Ma Yinghe; Li Zhiyu; (15 pag.)CN109574920; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 112734-22-2, 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. 112734-22-2, name is (4-Bromo-2-fluorophenyl)methanamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[0229] To a mixture of (4-bromo-2-fluorophenyl)methanamine (1.0 g, 4.9 mmol, 1.0 equiv) and IPA (15 mL) in a microwave vial (20 mL) were added 2-fluoropyrazine (0.58 g, 5.9 mmol, 1.2 equiv) and DIPEA (1.5 g, 11.8 mmol, 2.4 equiv). The vial was sealed and heated at 170 C in a microwave reactor for 4 h. The mixture was concentrated onto silica (10 g) and purified by silica gel chromatography (40 g column, 20-100% EtOAc/hexanes) to provide 0.82 g (59%) of /V-(4-bromo-2-fluorobenzyl)pyrazin-2-amine as a pale yellow solid. LRMS (ES) m/z 282.0 (M+H).

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-Bromo-2-fluorophenyl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CYTOKINETICS, INC.; MORGAN, Bradley P.; VANDERWAL, Mark; CHUANG, Chihyuan; (0 pag.)WO2020/5888; (2020); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 1198171-18-4 as follows. category: bromides-buliding-blocks

1-Bromo-2-(difluoromethyl)-4-fluorobenzene (Preparation 50, 772 mg, 3.43 mmol) and sodium ethanethiolate (352.7 mg, 3.77 mmol) in DMSO (5 mL) was heated at 50 C. for 18 hours. On cooling, water (70 mL) was added to the reaction mixture, the product was extracted with EtOAc (20 mL*3). The combined organic layers were concentrated to give the crude product, which was purified by silica gel column chromatography eluting with heptane to afford the title compound as a colourless oil (260 mg, 28%). 1H NMR (400 MHz, CDCl3): delta ppm 1.33 (3H, t), 2.98 (2H, q), 6.88 (1H, t), 7.25 (1H, d), 7.50 (1H, d), 7.56 (1H, s).

According to the analysis of related databases, 1198171-18-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfizer Limited; Omoto, Kiyoyuki; Owen, Robert McKenzie; Pryde, David Cameron; Watson, Christine Ann Louise; Takeuchi, Mifune; US2014/171435; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 2606-51-1, name is 5-(Bromomethyl)benzo[d][1,3]dioxole, 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 2606-51-1, Recommanded Product: 2606-51-1

Compound 1 (500 mg, 2.5 mmol) was dissolved in THF (tetrahydrofuran, 25 ml), followed by Na 2 SO 4 (7.09 g, 50 mmol) and piperral.(piperonal, 375 mg, 2.5 mmol) was added, and AcOH (0.2 ml) was added dropwise, followed by stirring at room temperature for 20 minutes. NaB (OAc) 3H(1.059 g, 5 mmol) was added, followed by stirring at room temperature for 16 hours, followed by addition of MeOH (5 ml) and stirring for 24 hours.I was. The reaction mixture was dissolved in DCM, 1N NaOH was added and extracted twice. The obtained organic layer was washed with brineAfter filtration, it was dried over anhydrous MgSO 4 and filtered. The filtrate was concentrated under reduced pressure, and then silica column chromatography.Prufied with (Mc: MeOH = 15: 1) to purify to afford a white solid compound 2-j (290 mg, 35%).

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, 5-(Bromomethyl)benzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Industry Academy Cooperation Foundation of Hanbat National University; Park Jeong-ho; Lee Seung-hwan; Kim Beom-cheol; Kim Jae-gwan; (24 pag.)KR101548927; (2015); B1;,
Bromide – Wikipedia,
bromide – Wiktionary