Extracurricular laboratory: Synthetic route of 399-94-0

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, 1-Bromo-2,5-difluorobenzene, other downstream synthetic routes, hurry up and to see.

Related Products of 399-94-0, 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. 399-94-0, name is 1-Bromo-2,5-difluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The reaction flask were sequentially added Compound 8 (386mg, 2.0mmol), Pd (OAc)2(18mg,4mol)dppp(66mg,8mol)DMSO(2mL)[bmim][BF 4] (2mL), allyl alcohol (0.27mL, 4.0mmol) and NEt3(0.42mL, 3mmol). The reaction mixture was stirred at 115 C 15 hours. After the reaction system was cooled to room temperature and extracted with dichloromethane, dried and the solvent was evaporated. Mixture was purified by column chromatography to give compound 9.

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, 1-Bromo-2,5-difluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Jiao Tong University; Zhang, yongjian; A, MAER; (10 pag.)CN104370939; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

The origin of a common compound about 1-Bromo-2,5-difluorobenzene

According to the analysis of related databases, 399-94-0, the application of this compound in the production field has become more and more popular.

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 399-94-0 as follows. 399-94-0

Under nitrogen, 2,5-difluorobromobenzene (15.05 g, 78 mmol) was dissolved in dry toluene (50 mL), the ice salt bath was cooled below -10 C,A solution of isopropylmagnesium chloride / lithium chloride tetrahydrofuran (66 mL, 1.3 mol / L) was added dropwise and the mixture was stirred at about -10 C for 1 hour.A solution of 1D (10 g, 39 mmol) in dry tetrahydrofuran (100 mL) was added dropwise to the reaction solution, maintaining the temperature at -10 C, and the reaction was carried out at room temperature for 4 hours.The temperature was lowered to about -10 C, saturated ammonium chloride solution (40 mL) was added dropwise, stirred for 10 minutes, adjusted to pH 5 to 6 with 3 mol / L hydrochloric acid solution,The aqueous phase was extracted with methyl tertiary butyl ether (50 mL x 2). The organic phases were combined, washed with saturated sodium chloride solution (30 mL x 2). The organic phase was dried over anhydrous sodium sulfate, filtered,Column chromatography (petroleum ether / ethyl acetate (v / v) = 50: 1-8: 1) gave a pale yellow solid 1E (10.1 g, yield 83.5%).

According to the analysis of related databases, 399-94-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sichuan Haisco Pharmaceutical Co.,Ltd; FAN, JIANG; CHEN, QINGPING; JIANG, WEI; ZHENG, SUXIN; YE, FEI; (128 pag.)TW2017/8221; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary