HRID325572

反应详情

EQUATION

反应方程式

HRID 325572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a slurry of 21.80 g. of 3-bromopropylamine hydrobromide in 200 ml. of glyme at 3° C. is added a solution of 23.9 g. of 2-(4-tetradecenylamino)benzoyl chloride hydrochloride in 65 ml. of glyme, concurrently with 26 ml. of triethylamine diluted to 39 ml. with 1,2-dimethoxyethane. The solution is warmed to reflux and 0.2 g. of 4-dimethylaminopyridine is added. The solution is heated for four hours and cooled overnight. The solid is removed and the mother liquor diluted with 200 ml. of water to yield a solid which is crystallized from cyclohexane and recrystallized from acetonitrile to yield the product.

WORKUP

后处理

  1. temperatureThe solution is warmed
  2. temperatureto reflux
  3. temperatureThe solution is heated for four hours
  4. temperaturecooled overnight
  5. customThe solid is removed
  6. additionthe mother liquor diluted with 200 ml
  7. customof water to yield a solid which
  8. customis crystallized from cyclohexane
  9. customrecrystallized from acetonitrile
  10. customto yield the product