反应详情

温度

22.5 °C

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 stating “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.

1. additionare added
2. customgradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals
3. filtrationThe crystals are collected by filtration
4. washwashed with methyl acetate
5. customdried