反応 #74949

反応方程式

chloromethylmethylether

chloromethylmethylether

N-(2-chloro-benzyl)-2-(2-thienyl)-ethylamine

water

→

5-(2-chloro-benzyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine hydrochloride

収率 148.9%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   workup.ADDITIONis added, over 7 minutes
2. 2
   温度the medium is cooled to 20° C
3. 3
   その他The desired product, which has precipitated out
4. 4
   ろ過is filtered
5. 5
   洗浄washed with 2×70 ml acetone

実験手順

To a solution of 50.8 g (0.2 M) N-(2-chloro-benzyl)-2-(2-thienyl)-ethylamine in 70 ml dimethylformamide heated at 60° C. is added, over 7 minutes, 22.7 g (0.24 M) chloromethylmethylether. The temperature of the reaction medium is maintained at 60° C. throughout the addition step by cooling with water. Thirty minutes after completion of the chloromethylmethylether addition, the medium is cooled to 20° C. The desired product, which has precipitated out, is filtered and washed with 2×70 ml acetone, to give 45.1 g 5-(2-chloro-benzyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine hydrochloride (Yield: 75%).

出典