反応 #1747831
ord-c5281949eec5411bb4c96d4f5176e287
反応方程式
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他to slowly rise to rt
- 2その他Evaporation of the volatiles
- 3その他gave a beige solid
- 4ろ過filtered
- 5その他to remove diethyl sulphite
- 6その他Recrystallization from dietyl ether
実験手順
To a cooled solution (−15° C.) of 3-aminophenylacetic acid (10.2, 67 mmol) in ethanol (200 mL) was added dropwise thionyl chloride (10 mL, 0.14 mol). The reaction mixture was stirred for 24 h allowing the temperature to slowly rise to rt. Evaporation of the volatiles gave a beige solid that was stripped several times with dichloromethane. The solid was then treated with hot diethyl ether and filtered to remove diethyl sulphite. Recrystallization from dietyl ether gave 14.4 g, 67 mmol, 100% of the desired compound as an off-white crystalline hydrochloride, mp 135° C. IR (KBr) cm−1 2857,2614, 1740