Month: June 2021

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. 5433-01-2, name is 1-Bromo-3-isopropylbenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 5433-01-2

Preparation Example 1-1: Preparation of 4-t-butyl-N- (4- isopropylphenyl ) benzenamine; As represented below in Reaction Scheme 1, 25g of 3-t- butylaniline (0.125mol) and 37.3g of 3-bromoisopropylbenzene(0.25mol) were dissolved in 25OmL of toluene, and 3.43g ofPd2(dba)3 (0.0037mol) was added thereto under a nitrogen atmosphere. Then, 14.4g of NaOBufc (0.15mol) and 1.157g of (t- Bu)3P (0.0075mol) were added to the reaction solvent, and the reaction mixture was refluxed and stirred for 12 hours. The reaction mixture was checked for the completion of the reaction by means of TLC, and if the reaction was completed, the reaction product was cooled down to room temperature. The reacted solution was poured onto a thin silica pad to perform short chromatography, and then was washed with methylene chloride (MC) . The washed solution was subjected to distillation under reduced pressure to thereby remove the solvent, and was chromatographed using n-hexane to thereby obtain a desired white solid product (29.4g, 88%). [Reaction Scheme 1]

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; DOOSAN CORPORATION; WO2009/91095; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 51376-06-8, name is 5-Bromobenzo[c][1,2,5]oxadiazole, 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 51376-06-8, Computed Properties of C6H3BrN2O

5-bromo-2,1,3-benzoxadiazole (0.71 g), cesium carbonate (1.4 g), 2,2′- bis(diphenylphosphino)-1,r-binapthyl (0.17 g) and Tris-(dibenzylideneacetone) dipalladium(O) (0.13g) were added to a solution of (5S)-3-[3-fluoro-4-(piperidin-4- yloxy)phenyl]-5-[(isoxazol-3-ylamino)methyl]-1,3-oxazolidin-2-one (1.3 g) (obtained from Step b) in dry dimethylformamide (15 mL) and the reaction mixture was heated at 100 C for about 17 hours. The reaction mixture was filtered and the solvent was evaporated. The crude product thus obtained was purified by column chromatography using 1 % methanol in dichloromethane to yield the title product (0.07g).Melting point: 75-100 C; EIMS (m/z): 534.21; 1HNMR(DMSO): delta 8.16 (s, 1H), 7.66 (d, 1H), 7.48 (dd, 1H), 7.3 (m, 2H), 7.17 (d, 1H), 7.08-7.05 (t, 1H), 6.75 (s, 1H), 4.99 (m, 1H), 4.53 (m, 3H), 4.14-4.11 (t, 1H), 3.95 (t, 1H), 3.61 (m, 2H), 3.3 (m, 2H), 2.04 (m, 4H).

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-Bromobenzo[c][1,2,5]oxadiazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; WO2006/35283; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 766-46-1, These common heterocyclic compound, 766-46-1, name is 2′-Bromophenylacetylene, 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: An oven dried 20 mL glass vial was charged with PdCl2(PPh3)2 (28.1 mg, 0.04 mmol), CuI (7.6 mg, 0.04 mmol), acid chloride (2.60 mmol), terminal alkyne (2.00 mmol) and anhydrous triethylamine (10 mL). The vial was flushed with nitrogen and sealed with a pressure relief cap. The reaction mixture was stirred at room temperature, overnight, until the disappearance of starting material was observed, as monitored by thin layer chromatography. The reaction mixture was diluted with diethyl ether (40 mL) and washed with brine (40 mL). The aqueous phase was then extracted with diethyl ether (2 x 20 mL). The combined organic layers were dried over anhydrous MgSO4, and concentrated using a rotary evaporator under reduced pressure (20 mmHg). The resulting residue was purified by flash column chromatography on silica gel (eluent: hexanes/ethyl acetate).

The synthetic route of 766-46-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Xiaochen; Hong, Dongsub; She, Zhigang; Hersh, William H.; Yoo, Barney; Chen, Yu; Tetrahedron; vol. 74; 45; (2018); p. 6593 – 6606;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 4263-52-9, A common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, molecular formula is C2H4BrNaO3S, 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: A solution of 1mmol of chloride salt 1a or 2a in distilled water was treated with equimolar quantity of various salts (NaBF4, KPF6, 2-BrCH2CH2SO3Na). The reaction mixture was stirred at room temperature for 12h. Next, the reaction mixture was extracted twice with CH2Cl2. The organic layer was dried over anhydrous Na2SO4 and then CH2Cl2 was evaporated on a rotary evaporator to give various chiral ionic liquids 1b-d and 2b-d. 4.4.6 1-[(-)-Borneoxycarbonylmethylene]-3-methyl benzimidazolium 2-bromoethylsulfonate [ABoMBI]OSO2CH2CH2Br 2d Off-white solid Yield = 83%, mp = 96-98 C, [alpha]D25 = -15.6 (c 0.25, EtOH). 1H NMR (CDCl3, 400 MHz): delta 10. 35 (s, 1H), 7.78-7.68 (d, 1H, Ar), 7.60 (s, 3H, Ar), 5.47 (s, 2H NCH2), 5.44-5.35 (d, 1 H), 4.13 (s, 3H N-CH3), 3.60-3.52 (t, 2H), 3.20-3.07 (t, 2H), 2.31-2.19 (m, 1H), 1.72-1.56 (m, 3H), 1.19 (s, 3H), 1.02-0.97 (d, 1H), 0.80 (s, 6H), 0.74 (s, 3H). 13C NMR (CDCl3, 400 MHz): delta 166.09, 144.39, 131.67, 131.47, 127.46, 127.32, 113.07, 112.93, 83.16, 54.40, 48.93, 47.91, 44.64, 36.34, 33.76, 29.59, 27.79, 26.87, 26.29, 19.58, 18.72, 13.47. EI-MS: m/z = 327 [M+cation], m/z = 312 [M+cation-CH3].

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; Singh, Avtar; Chopra, Harish Kumar; Tetrahedron Asymmetry; vol. 27; 11-12; (2016); p. 448 – 453;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 21524-34-5, name is 2-Bromo-1,3,5-triisopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Bromo-1,3,5-triisopropylbenzene

General procedure: Ligand comparison reactions were setup at the same time using the same batches of reagents. In a N2 filled glove-box, a microwave vialwas charged with a magnetic stir bar, Pd2(dba)3 (2.3 mg, 0.0025mmol), the respective ligand L1-L5 (0.010 mmol), K3PO4 (424 mg, 2.00 mmol), and 2-biphenyboronic acid (9; 158 mg, 0.800 mmol). Degassed (argon sparge) toluene (1.3 mL) followed by bromide 8 (0.169 mL, 0.667 mmol) were added, and the vial was sealed with acrimp-cap septum and removed from the glove-box. The reaction vialwas then inserted into a heating block pre-heated to 80 C. Aliquots were removed using argon-purged syringes and quenched into MeOH and analyzed by UPLC. After complete consumption of the starting aryl bromide (2 h), the reaction mixture was cooled to r.t. and partitioned between H2O and CH2Cl2. The organic layer was collected,dried (anhyd Na2SO4), and concentrated in vacuo. The yield of thecrude mixture was determined by 1HNMR spectroscopy using dimethyl fumarate as the analytical standard.

According to the analysis of related databases, 21524-34-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Yongda; Lao, Kendricks S.; Sieber, Joshua D.; Xu, Yibo; Wu, Linglin; Wang, Xiao-Jun; Desrosiers, Jean-Nicolas; Lee, Heewon; Haddad, Nizar; Han, Zhengxu S.; Yee, Nathan K.; Song, Jinhua J.; Howell, Amy R.; Senanayake, Chris H.; Synthesis; vol. 50; 22; (2018); p. 4429 – 4434;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 2550-36-9, 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. 2550-36-9, name is (Bromomethyl)cyclohexane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

20 g of bromomethyl cyclohexane,After 12.5 g of 1-naphthol was dissolved in 300 g of NMP in a three-necked flask,12g of potassium carbonate was added,14g potassium iodide was heated at 120 C for 8 hours.In the reaction solution was added 300g of water,Extraction was performed three times with 100 g of hexane,The resulting organic layers were combined,Washed once with 100 g of 1 N aqueous sodium hydroxide solution,Water 100g washed once,Brine 100g washed once,Concentration gave 13 g of compound 1.

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

Reference:
Patent; FUJIFILM CORPORATION; SHIRAKAWA, MICHIHIRO; TANGO, NAOHIRO; SHIBUYA, AKINORI; YAMAGUCHI, SHUHEI; KATAOKA, SHOHEI; (175 pag.)TWI579263; (2017); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 2606-51-1, 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. 2606-51-1, name is 5-(Bromomethyl)benzo[d][1,3]dioxole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 3 (870 mg, 3.36 mmol) in DMF (8 mL) was treated with 60% NaH dispersion in mineral oil (134 mg, 3.36 mmol) under N2. The mixture was stirred at r.t. for 10 min, then 4-(bromomethyl)-1-fluoro-2-methoxybenzene (700 mg, 3.20 mmol) was added. The resulting mixture was stirred at 20 C under N2 for 2 h. The mixture was diluted with H2O (80 mL) and extracted with EtOAc (80 mL). The organic layer was dried (MgSO4), filtered and evaporated. The crude product was purified by flash silica gel chromatography (eluent: gradient 20 to 25% EtOAc in heptane). Pure fractions were evaporated to dryness and dried under high vacuum to afford the title compound 4, containing 32 mol% EtOAc (1.20 g, 88%, allowing for solvent residues) as a colourless oil. 1H NMR (500 MHz, CDCl3): delta = 7.73 (d, J = 8.1Hz, 2 H), 7.31 (d, J = 8.1Hz, 2 H), 6.96 (dd, J = 11.1, 8.2 Hz, 1H), 6.82 (dd, J = 8.2, 2.1Hz, 1H), 6.71 (ddd, J = 8.2, 4.2, 2.1Hz, 1H), 4.42 (s, 2 H), 4.36 (t, J = 5.3 Hz, 1H), 3.78 (s, 3 H), 3.26 (s, 6 H), 3.21 (d, J = 5.3 Hz, 2 H), 2.43 (s, 3 H). 13C NMR (126 MHz, CDCl3): delta = 151.9 (J = 245.6 Hz), 147.7 (J = 11.0 Hz), 143.4, 137.5, 132.6 (J = 3.7 Hz), 129.7, 127.2, 120.9 (J = 6.8 Hz), 115.7 (J = 18.5 Hz), 113.4 (J = 1.7 Hz), 104.0, 56.1, 54.7, 52.3, 48.8, 21.5. MS (ES+): m/z = 334 [M + H – 2 MeOH]+. [CAS Reg. No. 1036711-00-8] A solution of 4 (1.18 g, 2.96 mmol) in 1,4-dioxane (12 mL) was treated with 6 N aq HCl (3.94 mL, 23.7 mmol) under N2. The resulting mixture was stirred under vigourous reflux for 24 h. The mixture was evaporated and the residue partitioned between EtOAc (50 mL) and 0.1 M aq NaHCO3 (70 mL). The aqueous layer was extracted with EtOAc (70 mL) and the extracts combined with the organic layer. The combined organic extracts were washed with sat. brine (50 mL), dried (Na2SO4), filtered and evaporated. The crude product was purified by flash silica gel chromatography (eluent: gradient 20 to 50% EtOAc in heptane). Pure fractions were evaporated to dryness to afford the title compound 17 (376 mg, 72%) as a beige solid

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:
Article; Pearson, Stuart E.; Fillery, Shaun M.; Goldberg, Kristin; Demeritt, Julie E.; Eden, Jonathan; Finlayson, Jonathan; Patel, Anil; Synthesis; vol. 50; 24; (2018); p. 4963 – 4981;,
Bromide – Wikipedia,
bromide – Wiktionary

10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, 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. name: 2,8-Dibromodibenzo[b,d]furan

250mL 2 necked flask equipped with a 10-phenyl-2 ‘- (4,4,5,5-tetra-methyl -1,3,2-dioxa-beam as is -2 yl) -10H- spiro [acridine -9,9’- fluorene] (3g, 5.62mmol), 2,8- di-bromo-modify-benzo [b, d] furan (2,8-dibromodibenzo [b, d] furan) (0.95 g, 2.25 mmol) , tetrakis (triphenylphosphine) palladium (0) (0.13g, 0.112 mmol), potassium carbonate (1.5g, 11.2mmol), tetrahydrofuran: water (3: 1) is dissolved in the mixture was stirred under reflux.After 12 hours After cooling to room temperature, extracted with dichloromethane, and then after drying the water with magnesium sulfate to remove the solvent.Hexane: ethyl acetate (10: 0.5) and the column with the solvent, to filter the resulting solid was precipitated with petroleum ether to give a white solid Compound B 1.5g (68% yield)

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

Reference:
Patent; LG DISPLAY CO., LTD.; Bae, Sook Young; Song, In Bum; Yun, Gyung Jin; Lee, Sang Ho; Noh, Hyo Jin; Yun, Dae Wei; Haw, Hay Ryong; Kim, Chun Gi; (17 pag.)KR2015/65385; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 68322-84-9, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows.

Intermediate 8: Preparation of 5-Cyano-5-(4-methoxy-8-trifluoromethyl- dibenzofuran-l-yl)-2-oxo-cyclohexanecarboxylic acid methyl esterStep-1: Preparation of 3-(2-Bromo-4-trifluoromethyl-phenoxy)-4-methoxy- benzaldehydeTo a stirred solution of Isovanillin (5 gm, 0.0328 moles) and Potassium carbonate (13.6 gm, 0.0985 moles) in dry DMF (20 ml) was added 3-Bromo-4- Fluorobenzotrifluoride (8.065 gm, 0.0331 moles) over a period of 15 min at room temperature under nitrogen atmosphere, and then above reaction mixture was stirred at 14O0C for 5 hrs. After completion of reaction, the reaction mixture was cooled to room temperature and the contents were poured in to water (100 ml) and extracted with ethyl acetate (3XlOOmI). The organic extracts were combined and washed with IN sodium hydroxide, water and brine, dried with sodium sulfate, filtered and solvent evaporated under vacuum to obtain the title compound (11.58 gm, yield-94%) a pale yellow solid.1H NMR (300 MHz, CDCl3) delta 3.92 (s, 3H), 6.75 (d, J= 8.6 Hz, IH), 7.15 (d, J= 8.5 Hz, IH), 7.45 (d, J= 8.6 Hz, IH), 7.54 (d, J = 1.9 Hz, IH), 7.77 (dd, J=8.4 Hz, J=I.9Hz, IH,), 7.90 (s, IH), 9.87 (s, IH)MS (M++.): 376

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MATRIX LABORATORIES LTD.; WO2009/115874; (2009); A2;,
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