HRID128514

反应详情

EQUATION

反应方程式

HRID 128514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

48.0 g (0.5 mol) of maleimide are initially introduced into the reaction vessel as a solution in 200 ml of absolute tetrahydrofuran, and 120 g (0.5 mol) of approximately 70% strength 1-(tert.-butyloxycarbonylamino)-1,3-butadiene are added dropwise as a solution in 500 ml of absolute tetrahydrofuran, the temperature being kept at 20° to 30° C. The mixture is subsequently stirred overnight at room temperature. It is then concentrated and the residue is recrystallised from ethyl acetate. 57 g of product having a melting point of 177° to 182° C. are obtained. A further 13 g of melting point 158° to 160° C. are obtained from the mother liquor.

WORKUP

后处理

  1. custombeing kept at 20° to 30° C
  2. concentrationIt is then concentrated
  3. customthe residue is recrystallised from ethyl acetate
  4. customare obtained
  5. customA further 13 g of melting point 158° to 160° C. are obtained from the mother liquor