反応 #411067

反応方程式

hydrochloride

methanol

methyl acetate

hydrogen chloride

[2-(2-thienyl)ethylamino](2-chlorophenyl)acetonitrile

→

[2-(2-thienyl)ethylamino](2-chlorophenyl)acetamide hydrochloride

反応条件

後処理

1. 1
   その他gradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals
2. 2
   ろ過The crystals are collected by filtration
3. 3
   洗浄washed with methyl acetate
4. 4
   その他dried

実験手順

Into 1200 ml of methyl acetate 204 g (5.6 mol) of hydrogen chloride gas is introduced at 15-25° C., and to the solution 221.4 g (0.8 mol) of the [2-(2-thienyl)ethylamino](2-chlorophenyl)acetonitrile of formula (I), prepared as described in Example 1., and 48 ml (1.2 mol) of methanol are added and the mixture is stirred at 20-25° C. for 6 hours. In the course of the reaction first the hydrochloride of the starting “nitrile”, then gradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals. The crystals are collected by filtration, washed with methyl acetate and dried. Weight: 249 g (94%) mp.: 231-232° C.

出典