Category: 1250444-23-5

Synthetic Route of 1250444-23-5,Some common heterocyclic compound, 1250444-23-5, name is 3-Bromo-2,6-difluorobenzonitrile, molecular formula is C7H2BrF2N, 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.

A mixture of 3- bromo-2,6-difluorobenzonitrile (4.4 g, 20 mmol), potassium ethanethioate (2.88 g, 25 mmol), Pd2(dba)3 (0.555 g, 0.61 mmol) and Xantphos (0.70 g, 1.2 mmol) in p-dioxane (30 mL) was stirred at 102 C for 15 hours. After cooling to ambient temperature, 28% aqueous ammonium hydroxide (12.3 g, 202 mmol) was added. The mixture was stirred at ambient temperature for 1 hour. Water (50 mL) and 2: 1 MTBE/hexanes (200 mL) were added. The aqueous layer was separated, acidified with 1 N HC1 to pH~5 and extracted with MTBE (50 mL). The organic layer was separated, washed with brine, dried (sodium sulfate), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel eluting with 3: 1 hexane/CH2Cl2 to give 2,6-difluorG-3-mercaptobenzonitrie (0.74 g, 21 %) as solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Bromo-2,6-difluorobenzonitrile, its application will become more common.

Reference:
Patent; PELOTON THERAPEUTICS, INC.; DIXON, Darryl, David; GRINA, Jonas; JOSEY, John, A.; RIZZI, James, P.; SCHLACHTER, Stephen, T.; WALLACE, Eli, M.; WANG, Bin; WEHN, Paul; XU, Rui; YANG, Hanbiao; WO2015/35223; (2015); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Reference of 1250444-23-5, 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. 1250444-23-5, name is 3-Bromo-2,6-difluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

3-bromo-2,6-difluorobenzonitrile and triethyl phosphite were fed at a ratio of 1: 8.0, N2 was protected, reacted The temperature is 100 C and the reaction is carried out under light conditions. TLC was monitored and reacted for 30 h until the feed point disappeared. The product is decompressed Distillation, the oil bath temperature to 10 C, steaming low boiling point fraction. The product was again subjected to vacuum distillation at an oil bath temperature of 190 C and steamed A high boiling fraction is taken and the fraction is taken at a temperature of 135-145 C. The distillate is dissolved in ethyl acetate and treated with 10% Na2C03, saturated sodium chloride, washed with anhydrous magnesium sulfate, filtered and evaporated to give a yellow oily liquid product in 83% yield.

The chemical industry reduces the impact on the environment during synthesis 3-Bromo-2,6-difluorobenzonitrile. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Tianjin Normal University; Song, fanbo; Zhang, ZhongBiao; Li, huayun; Tang, hongying; Wang, ZhiJiang; Song, AiRu; (8 pag.)CN104017021; (2016); B;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

These common heterocyclic compound, 1250444-23-5, name is 3-Bromo-2,6-difluorobenzonitrile, 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. 1250444-23-5

3-bromo-2,6-difluorobenzonitrile and triethyl phosphite in a 1: 8.0 proportion feeding, N2 Protection, reaction temperature 100 , reaction was carried out under the lighting conditions. TLC monitored the reaction to the raw material 30h point disappears. The product was distilled under reduced pressure, the oil bath temperature to 100 deg.] C, the low boiling fraction was distilled off. Again the product distilled under reduced pressure, the oil bath temperature to 190C, distilled high boiling fraction, taken when the steam temperature 135-145C fraction, the evaporated fraction dissolved in ethyl acetate, respectively, with 10% Na2CO3, Washed with saturated sodium chloride, dried over anhydrous magnesium sulfate, filtered and rotary evaporated to give a yellow oily liquid product, in 83% yield.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1250444-23-5.

Reference:
Patent; Tianjin Normal University; SONG, FANBO; ZHANG, ZHONGBIAO; LI, HUAYUN; TANG, HONGYING; WANG, ZHIQIANG; SONG, AIRU; (11 pag.)CN104004016; (2016); B;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts