HRID222244
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 mixture of 1-tert-butyl 4-ethylpiperidine-1,4-dicarboxylate (21 g), hydrazine monohydrate (40 mL), and ethanol (200 mL) was heated and refluxed for 22 hours. After leaving to be cooled, the solvent was evaporated under reduced pressure, to the residue were added saturated brine and ethyl acetate, and the organic phase was separated. The organic phase was dried over magnesium sulfate and the solvent was evaporated under reduced pressure. To the residue was added diisopropyl ether, followed by stirring for 1 hour, and the resulting solid was collected by filtration and dried under reduced pressure to obtain tert-butyl 4-(hydrazinocarbonyl)piperidine-1-carboxylate (17.8 g).
WORKUP
后处理
- temperaturewas heated
- temperaturerefluxed for 22 hours
- customAfter leaving
- temperatureto be cooled
- customthe solvent was evaporated under reduced pressure, to the residue
- additionwere added saturated brine and ethyl acetate
- customthe organic phase was separated
- dry with materialThe organic phase was dried over magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- additionTo the residue was added diisopropyl ether
- filtrationthe resulting solid was collected by filtration
- customdried under reduced pressure