4333-56-6

1759-53-1

4333-56-6

(1) 179 g of 1,3-bromochloropropane was added to a three-necked flask, 29 g of potassium cyanide and 50 ml of water were added and heated and stirred until completely dissolved. Subsequently, 70 ml of ethanol solution was added and the mixture was stirred and refluxed for 2 hours. After completion of the reaction, it was cooled to room temperature and diluted with 300 ml of water to separate the oil and aqueous phases. The aqueous phase was extracted with 40 ml of chloroform, the organic phases were combined and dried with anhydrous calcium chloride. 316.9 g of hydrogen chloride was obtained. Chlorobutanenitrile 241.6 g was prepared by adding 100 ml of sodium hydroxide solution and stirring the reaction for 2 hours. Then 200 ml of water was added, cooled to about 10°C, 44 ml of concentrated sulfuric acid was added to acidify the reaction mixture, extracted with petroleum ether as an extractant, the organic phases were combined and dried with anhydrous sodium sulfate to obtain 330.1 g of cyclopropionic acid. (2) 324.8 g of cyclopropionic acid was added dropwise to a reaction flask with 48 g of mercuric oxide, 160 ml of a mixture of 1,1,2,2-tetrachloroethane and 64.4 g of liquid bromine, and stirred for 2 hours. After completion of the reaction, the mixture was cooled to 5°C, washed with tetrachloroethane and then dried with calcium chloride to give 419.15 g of bromocyclopropane.