HRID1449070

反应详情

EQUATION

反应方程式

HRID 1449070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 15.9 g of ethyl-β-amino-β-ethoxy acrylate in 60 ml of benzene was added 10.3 g of triethylamine, and a solution of 11.5 g of methanesulfonyl chloride in 40 ml of benzene was dropped thereinto with stirring. After the dropping, the resulting mixture was stirred at room temperature for 5 hours. The crystals formed were separated. The filtrate was concentrated under reduced pressure and the concentrated residue crystallized by cooling. When the crystals were washed with n-hexane and dried, 16 g of prismatic crystals of a melting point of 103° to 104° C. was obtained.

WORKUP

后处理

  1. stirringAfter the dropping, the resulting mixture was stirred at room temperature for 5 hours
  2. customThe crystals formed
  3. customwere separated
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe concentrated residue crystallized
  6. temperatureby cooling
  7. washWhen the crystals were washed with n-hexane
  8. customdried