HRID874762

反应详情

EQUATION

反应方程式

HRID 874762 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of hydrazine (3 mL) and tert-butyl(3Z)-3-[(dimethylamino)methylene]-4-oxopyrrolidine-1-carboxylate (19.22 g) in ethanol (40 mL) was heated at 85° C. in a sealed tube for 4 h. Solvent was removed under reduced pressure, and the residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL). The resulting solid was filtered. The filtrate was concentrated and the resulting solid was triturated again and filtered. The combined solids were used without further purification. LC/MS: 210.1 (M+1).

WORKUP

后处理

  1. customSolvent was removed under reduced pressure
  2. customthe residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL)
  3. filtrationThe resulting solid was filtered
  4. concentrationThe filtrate was concentrated
  5. customthe resulting solid was triturated again
  6. filtrationfiltered
  7. customThe combined solids were used without further purification