HRID651976

反应详情

EQUATION

反应方程式

HRID 651976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 1.0 grams of N2 -dansyl-L-arginine and 1.4 gram of p-toluenesulfonic acid monohydrate in 10 ml of benzyl alcohol was heated for 30 minutes at 100° C. To the thus obtained clear solution, 100 ml of benzene was added, and the mixture was refluxed for 5 hours, removing water by azeotropic distillation. After the solvent was removed by distillation, 100 ml of ethyl ether was added to the residue, giving a crystalline mass. Crystallization from acetone gave N2 -dansyl-L-arginine benzyl ester di(p-toluenesulfonate) in 87% yield; mp. 150°-153° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 5 hours
  2. customremoving water
  3. distillationby azeotropic distillation
  4. customAfter the solvent was removed by distillation, 100 ml of ethyl ether
  5. additionwas added to the residue
  6. customgiving a crystalline mass
  7. customCrystallization from acetone