HRID46676

反应详情

EQUATION

反应方程式

HRID 46676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

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%).

WORKUP

后处理

  1. additionis added, over 2 minutes
  2. additionThe reaction is exothermal and, during the addition
  3. customthe reaction
  4. temperatureto maintain the temperature of the reaction medium below 70° C
  5. additionAfter completion of the addition
  6. temperaturethe material is then cooled
  7. filtrationThe desired product is filtered off
  8. washwashed twice with acetone