Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 460-00-4, name is 1-Bromo-4-fluorobenzene, 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 460-00-4, Recommanded Product: 460-00-4

Under nitrogen protection,Add carbazole (5 g, 30 mmol) to a 250 mL single-necked flask,P-fluorobromobenzene (10.47g, 60mmol),Cesium carbonate (21.5 g, 62 mmol) was mixed in dimethyl sulfoxide DMSO (100 mL).Reacted at 160 C for 48 hours,Cool to room temperature, extract with dichloro/water solution, and pass through the column with dichloromethane/petroleum ether.After drying in vacuo, 7.7 g of white crystals were obtained.The yield was 80%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4-fluorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Jilin University; Zhang Ming; Zhang Zhaoxia; (27 pag.)CN109988097; (2019); A;,
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. 4333-56-6, name is Bromocyclopropane, This compound has unique chemical properties. The synthetic route is as follows., name: Bromocyclopropane

Intermediate 54: (2S)-Lambda/-r(S)-cvclopropyl(phenv?methyll-3-methyl-1-r(trimethylsilyl)oxyl- 2-butanamine; EPO Cyclopropyl bromide (4.64g, 38.4mmole) was dissolved in dry Et2O (50ml) under argon, cooled to -780C and treated with tert-BuLi (45ml_ of a 1.7M solution in pentane, 76.5mmole). After 10 minutes, cooling was removed and the mixture stirred at room temperature for 1 hr. After re-cooling to -4O0C, a solution of Intermediate 52 (8.43g, 32mmole) in dry Et2O (40ml) was added and stirring continued at -4O0C for 1.5 hrs. 5M HCI acid was added (50ml) and the phases separated. The aqueous phase was washed with Et2O (discarded) and then basified with KOH pellets to pH >10 in the presence of Et2O. The organic phase was washed with water and brine and then evaporated to dryness under vacuum to afford the title compound as a colourless oil (6.42g, 86%); 1 HNMR (400MHz, CDCI3) delta 0.13 – 0.15, (1 H, m), 0.34 – 0.37, (2H1 m), 0.60 – 0.70, (1 H, m), 0.83, (3H, d, J = 7Hz), 0.91 , (3H, d, J = 7Hz), 0.98 – 1.00, (1 H, m), 1.71 – 1.77, (1 H, m), 2.44 – 2.48, (1 H, m), 3.00, (1 H, d, J = 8Hz), 3.32 and 3.36, (1 H, dd, J = 5 and 11 Hz), 3.59 and 3.61 , (1 H, dd, J = 5 and 11 Hz), 7.25 – 7.42, (5H, m); m/z(APCI): 234.2 [M+H]+.

According to the analysis of related databases, 4333-56-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2006/50992; (2006); 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. 5003-71-4, name is 3-Bromopropan-1-amine hydrobromide, A new synthetic method of this compound is introduced below., Product Details of 5003-71-4

Di-tert-butyl dicarbonate (1.01 g, 4.6mmol) was dissolved in N,N-dimethylacetamide (12ml) and added with 3-bromoaminopropane hydrobromide (1.01 g, 4.6mmol) and potassium carbonate(0.64 g, 4.6mmol). The reaction was carried out at 45-50C for 1 hour. 2-(5-Nitropyridine-2-yl)phenol(0.50 g, 2.3mmol) synthesized in Example 63 (i) and potassium carbonate (0.64 g, 4.6mmol) were added. The reaction was carried out at 50C for 20 minutes and at 75-80C for 1 hour. The reaction was cooled and extracted with addition of water and ethyl acetate. The organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure. The precipitated crystals were filtered with addition of water. The resulting crystals were dissolved in methanol, and hydrolyzed with dropwise addition of hydrochloric acid at 50C. The solution was concentrated and neutralized with saturated aqueous sodium bicarbonate. The precipitated crystals were filtered to give the title compound (0.57 g, 66.4%).

The synthetic route of 5003-71-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daito Chemix Corporation; Kyoto University; KAKIZUKA, Akira; HORI, Seiji; SHUDO, Toshiyuki; FUCHIGAMI, Tomohiro; EP2599771; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1422-54-4, 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. 1422-54-4, name is 2-Bromo-6-fluorotoluene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 187 6-(3-Fluoro-2-methylphenyl)-1,2-dihydro-2,2,4-trimethylquinoline (Compound 287, structure 4 of Scheme II, where R1 =3-fluoro-2-methylphenyl) This compound was prepared by General Method 2 (EXAMPLE 9) from Compound 9 (50 mg, 0.158 mmol) and 2-bromo-6-fluorotoluene (60 mg, 0.315 mmol). Purification by flash chromatography on silica gel (20g) using 5% EtOAc:hexanes afforded 6 mg(14%) of Compound 287 as a yellow oil. Data for Compound 287: 1 H NMR (400 MHz, acetone-d6) 7.20 (m, 1H), 7.02 (m, 1H), 6.98 (m, 2H), 6.91 (m, 1H), 6.56 (d, J=8.0, 1H), 5.37 (s, 1H), 5.37 (s, 1H), 5.29 (br s, 1H), 2.19 (s, 3H), 1.98 (s, 3H), 1.28 (s, 6H).

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, 2-Bromo-6-fluorotoluene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5693647; (1997); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 58534-95-5, These common heterocyclic compound, 58534-95-5, name is 3-Bromo-2-fluoroaniline, 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.

To a stirred solution of N-Boc-trans-4-fluoro-proline (25 g, 1 equiv), 3-bromo-2- fluoroaniline (14.5 mL, 1.2 equiv) and HATU (53 g, 1.3 equiv) in DMF (250 mL) was added DIPEA (37 mL, 2 equiv) and the resulting solution was stirred at room temperature under an atmosphere of nitrogen. The reaction mixture was poured into water and filtered and the collected solid was washed with excess water. The solid was dissolved in DCM and washed with 10% NaHCCb, 1.5 N HC1, and brine. The solvent was removed under vacuum, hexane was added, and the precipitated solid was collected by filtration to afford the title product (27 g).

Statistics shows that 3-Bromo-2-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 58534-95-5.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAL, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; GREENLEE, William; (447 pag.)WO2017/35408; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 58534-95-5, name is 3-Bromo-2-fluoroaniline, 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 58534-95-5, Product Details of 58534-95-5

[0179] To a solution of 3-bromo-2-fluoroaniline (0.5 g, 2.63 mmol) in Pyridine (20 mL) was added propane-1-sulfonyl chloride (3.75 g, 26.3 mmol) at rt, the reaction was stirred at 60C for 3h under N2, after the reaction was completed, the solvent was removed. The residue was purified on silica gel column chromatography (PE/EtOAc = 10/1) to afford N-(3- bromo-2-fluorophenyl)propane-1-sulfonamide (364 mg, 47% yield) as a yellow solid (the product has no MS).

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, 3-Bromo-2-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ABM THERAPEUTICS, INC.; CHEN, Chen; (154 pag.)WO2019/60611; (2019); 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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1-Bromo-3,4,5-trifluorobenzene

5-Bromo-1,2,3-trifluorobenzene (19.855 g, 94.110 mmol) was added slowly dropwise to a chilled (-85 to -80 C. (liquid nitrogen/acetone)) solution of n-butyllithium (9.10 mL, 2.38 M, 21.7 mmol combined with 45.5 mL, 1.57 M, 71.4 mmol; total: 93.1 mmol) in ether (200 mL) such that the temperature did not exceed -89 C. The temperature was allowed to increase to between -78 and -75 C. for 2.5 hours (dry ice bath) with formation of white precipitate. The reaction mixture was cooled to -85 C. A solution of dimethylphosphoramidous dichloride (6.791 g, 46.53 mmol) in ether (10 mL) was added very slowly dropwise such that the temperature did not exceed -80 C. Dry ice was added to the bath and the reaction mixture was allowed to stir overnight while warming to ambient temperature. 31P and 19F NMR spectra showed the product to be about 99.5% desired product. The reaction mixture was filtered and the volatiles were removed under reduced pressure. The residue was extracted with hexane, filtered, and the volatiles were removed under reduced pressure to give 5 as a pale yellow oil, 13.50 g, 86.04%. 1H NMR (500 MHz, CDCl3) delta 6.95 (dt, J=7.5, 6.4 Hz, 4H), 2.64 (d, J=9.7 Hz, 6H). BC NMR (101 MHz, CDCl3) delta 151.35 (dddd, J=254.1, 10.0, 8.2, 3.0 Hz), 140.00 (dtd, J=254.5, 15.5, 2.2 Hz), 134.44 (dq, J=21.9, 3.7 Hz), 115.41 (ddd, J=21.7, 15.1, 5.5 Hz), 41.47 (d, J=16.3 Hz). 31P NMR (202 MHz, CDCl3) delta 65.05. 19F NMR (376 MHz, CDCl3) delta -133.39–133.55 (m), -159.17 (ttd, J=20.3, 6.7, 3.4 Hz).

The synthetic route of 138526-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dow Global Technologies LLC; Klosin, Jerzy; Milbrandt, Kara A.; Boelter, Scott D.; Wilson, David R.; Rosen, Mari S.; Welsh, Dean M.; Margl, Peter M.; Koh, Kyoung Moo; Pearson, David M.; Huacuja, Rafael; (191 pag.)US2018/291048; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 960203-41-2, name is (2-Bromophenyl)(2,4-dimethylphenyl)sulfane, 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 960203-41-2, HPLC of Formula: C14H13BrS

In a 200 ml reaction flask,Compound 6 (5.8 g, 20 mmol) was added,Piperazine (2.1 g, 24 mmol),N-diisopropylethylamine (DIEA) (5.17 g) and 75 ml of DMF,Stirring to dissolve,Another cuprous iodide (0.4 g) was added,The reaction was carried out at 80 ° C for 10 hours,After completion of the reaction, the temperature was lowered to room temperature,The reaction solution was concentrated,And extracted three times with dichloromethane / water (V: V)The aqueous layer was washed once with dichloromethane,The combined organic phases were dried over anhydrous sodium sulphate,And concentrated to obtain 5.0 g of the compound (7) in a yield of 84.6percent

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; Shandong Kangmeile Pharmaceutical Technology Co., Ltd.; Geng, Fengluan; Fan, Mingwei; Liu, Yunfeng; Yuan, Zengfei; Liu, Xiaojun; (8 pag.)CN105985301; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 138526-69-9, 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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Set the reflux reaction device, put the stirrer into the reaction flask, Adding 4-pentylbiphenylboronic acid, 1,2-difluoro-4-bromobenzene, catalyst Pd (Pph3) 4, sodium carbonate; Sealing the reaction system, replacing the air in the sealing system into nitrogen; Immediately add isopropanol and water, stir and slowly heat reflux to ensure that the system reacts under nitrogen. After 5 hours, the degree of reaction was measured with TLC.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-3,4,5-trifluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Shenzhen Chao Duowei Optoelectric Zi Co., Ltd.; Shenzhen Mokerui Optoelectric Zi Institute; Zhang Guoxian; Bao Rui; (19 pag.)CN106397288; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 876-53-9,Some common heterocyclic compound, 876-53-9, name is 1,3-Dibromoadamantane, molecular formula is C10H14Br2, 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.

Compound 1,3-dibromo-adamantane (3 g, 10 mmol) was dissolved in 30 mL of toluene, and then 250 mg of AIBN (1.5 mmol), 7 g of tri-n-butyl tin (24 mmol), 3 g of ethyl acrylate (30 mmol) were added in order. The reaction was refluxed with at 110 C. under nitrogen for 3 hours. The reaction solution was cooled to room temperature and was poured into 30 mL of 0.2M aqueous ammonia. After being stirred fully, the organic layer was separated. The aqueous layers were extracted with ethyl acetate (20 mL×4). The organic layers were combined and washed with 30 mL of water and 30 mL of saturated sodium chloride solution. The resulting materials were dried with anhydrous sodium sulfate, and solvent was evaporated under the reduced pressure to give a crude product as a colorless oil, which was separated by silica column chromatography (petroleum ether:ethyl acetate=10:1) to give compound NM-011a as a colorless oil (2 g, 46.6%). ESI-MS: m/z 337.4 ([M+H]+). 1H-NMR (DMSO-d6, ppm): 1.11 (s, 2H), 1.15-1.19 (m, 6H), 1.28-1.39 (m, 12H), 1.53 (s, 2H), 1.97 (s, 2H), 2.19-2.24 (m, 2H), 4.03 (q, 4H, J=7.1 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromoadamantane, its application will become more common.

Reference:
Patent; Guangzhou Magpie Pharmaceuticals Co., Ltd.; Wang, Yuqiang; Liu, Zheng; Yu, Pei; Sun, Yewei; Zhang, Zaijun; Zhang, Gaoxiao; Shan, Luchen; Yi, Peng; Larrick, James; (19 pag.)US2018/148404; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary