HRID234614
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
Hydrazine monohydrate (65 ml) was added dropwise to a solution of methyl 1-methyl-1H-pyrrole-2-acetate (0.326 mol) in ethanol (300 ml) and the mixture was refluxed for 4 hours. The mixture was evaporated till dryness. The residue was taken up in dichloromethane and an aqueous potassium carbonate solution (10%) and extracted with dichloromethane. The organic layer was dried (MgSO4) and evaporated. The residue (48.8 g) was taken up in 1,1'-oxybisethane and the precipitate was filtered off, yielding 45.3 g (90%) of 1-methyl-1H-pyrrole-2-acetic acid, hydrazine (interm. 7).
WORKUP
后处理
- temperaturethe mixture was refluxed for 4 hours
- customThe mixture was evaporated till dryness
- extractionan aqueous potassium carbonate solution (10%) and extracted with dichloromethane
- dry with materialThe organic layer was dried (MgSO4)
- customevaporated
- filtrationthe precipitate was filtered off