反应 #4291

反应方程式

N-[2-[(3,4-dichlorophenyl)sulfonyl]ethyl]-N-(1-methylethyl)carbamic acid phenyl ester

→

white crystalline product

收率 32.4%

N-[2-[(3,4-Dichlorophenyl)sulfonyl]ethyl]-2-propanamine

收率 32.4%

溶剂

HBr

反应条件

后处理

1. 1
   温度at reflux for 12 hr
2. 2
   萃取extracted with chloroform
3. 3
   萃取The chloroform layer was extracted with 1N sulfuric acid
4. 4
   萃取The sulfuric acid layer was extracted with chloroform
5. 5
   其他evaporated to an oil
6. 6
   其他A portion of the oil was reacted with ethereal hydrogen chloride

实验过程

A solution of 44.27 g (0.107 mole of N-[2-[(3,4-dichlorophenyl)sulfonyl]ethyl]-N-(1-methylethyl)carbamic acid phenyl ester in 300 ml of 48% HBr was heated at reflux for 12 hr. The reaction mixture was cooled to room temperature, made alkaline with 50% sodium hydroxide-ice and extracted with chloroform. The chloroform layer was extracted with 1N sulfuric acid. The sulfuric acid layer was extracted with chloroform and the chloroform layers combined and evaporated to an oil, the free base of the title compound. A portion of the oil was reacted with ethereal hydrogen chloride to give an overall yield of 32.4% white crystalline product, m.p. 219°-221° C.

来源