反応 #74954

反応方程式

chlorobenzylamine

hydrochloric acid

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

hexahydrotriazine

→

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

溶媒

dimethylformamide

water

反応条件

後処理

1. 1
   workup.ADDITIONis added, over 2 minutes
2. 2
   workup.ADDITIONThe reaction is exothermal and, during the addition
3. 3
   その他the reaction
4. 4
   温度to maintain the temperature of the reaction medium below 70° C
5. 5
   workup.ADDITIONAfter completion of the addition
6. 6
   温度the material is then cooled
7. 7
   ろ過The desired product is filtered off
8. 8
   洗浄washed twice with acetone

実験手順

To 42 ml dimethylformamide in which are dissolved 0.25 mole gaseous hydrochloric acid and heated at 40° C. is added, over 2 minutes, a mixture of 25.15 g (0.1 M) N-(2-chloro-benzyl)-2-(2-thienyl)ethylamine and 15.3 g (0.033 M) s.hexahydrotriazine of o.chlorobenzylamine. The reaction is exothermal and, during the addition, the reaction must be cooled with water to maintain the temperature of the reaction medium below 70° C. After completion of the addition, stirring is continued for a further 30 minutes and the material is then cooled. The desired product is filtered off and washed twice with acetone, to give 17.3 g 5-(2-chloro-benzyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine hydrochloride. Treatment of the filtrates provides another 20 g of the desired product (Overall yield: 90%).

出典