反応 #521352
ord-12931a982b2c46bda5dc1e14be940140
反応方程式
methanol
hydrochloride
methyl acetate
hydrogen chloride
[2-(2-thienyl)ethylamino](2-chorophenyl)acetonitrile
→
[2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide Hydrochloride
反応物
試薬
なし
反応条件
温度
22.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他prepared
- 2その他gradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals
- 3ろ過The crystals are collected by filtration
- 4洗浄washed with methyl acetate
- 5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 are added 221.4 g (0.8 mol) of the [2-(2-thienyl)ethylamino](2-chorophenyl)acetonitrile, prepared as described in Example 1., and 48 ml (1.2 mol) of methanol. 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.