HRID874762
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customSolvent was removed under reduced pressure
- customthe residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL)
- filtrationThe resulting solid was filtered
- concentrationThe filtrate was concentrated
- customthe resulting solid was triturated again
- filtrationfiltered
- customThe combined solids were used without further purification