反応 #4288

反応方程式

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

isopropylamine

→

title compound

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

反応条件

後処理

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

実験手順

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.

出典