反应 #4288

反应方程式

methanesulfonic acid[2-[(3,4-dichlorophenyl)thio]ethyl]ester

isopropylamine

→

title compound

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

反应条件

后处理

1. 1
   其他The isopropylamine was removed in a rotary evaporator
2. 2
   其他the residue partitioned between chloroform and 5% sodium hydroxide
3. 3
   其他The chloroform was removed by rotary evaporator
4. 4
   其他to give an oil

实验过程

A solution of 151.46 g (0.548 mole) of methanesulfonic acid[2-[(3,4-dichlorophenyl)thio]ethyl]ester in 100 ml of isopropylamine was heated overnight in a bomb at 100° C. The isopropylamine was removed in a rotary evaporator and the residue partitioned between chloroform and 5% sodium hydroxide. The chloroform was removed by rotary evaporator to give an oil, the free base of the title compound. The oil was dissolved in methanol and converted to the hydrochloride salt with ethereal hydrogen chloride. Recrystallization of the salt from methanol-diethyl ether gave 101.53 g (61.6%) of white crystalline product, m.p. 132°-133.5° C.

来源