HRID1699601

反应详情

EQUATION

反应方程式

HRID 1699601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

30.0 g of N-(p-toluenesulfonyl)-alanine and 6 to 7 drops of DMF (dimethylformamide) were dissolved in 100 ml of dichloromethane and 5 ml of oxalyl chloride was added dropwise. After stirring for 3 hours at room temperature the reaction mixture was evaporated down to a residue which was dissolved in 100 ml of dichloromethane. The dichloromethane was again evaporated and the resulting residue dissolved in 50 ml of dichloromethane followed by the addition of 100 ml hexane. After standing in the refrigerator overnight the crystals, so formed, were filtered and dried.

WORKUP

后处理

  1. customwas evaporated down to a residue which
  2. dissolutionwas dissolved in 100 ml of dichloromethane
  3. customThe dichloromethane was again evaporated
  4. dissolutionthe resulting residue dissolved in 50 ml of dichloromethane
  5. additionfollowed by the addition of 100 ml hexane
  6. customAfter standing in the refrigerator overnight
  7. customso formed
  8. filtrationwere filtered
  9. customdried