HRID713410
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
To a stirred solution of 4-hydrazinocarbonyl-piperidine-1-carboxylic acid tert-butyl ester (1.15 g, 4.73 mmol, 1.0 eq) in EtOH (15 mL) was added benzimidic acid ethyl ester hydrochloride (921 mg, 4.96 mmol, 1.05 eq.) and the reaction mixture was refluxed for 48 h. The inorganic precipitate was filtered off, washed with ethyl acetate, and the solvent of the mother liquor was evaporated in vacuo. The residue was purified by column chromatography (ethyl acetate/heptanes) to give the title compound as a white solid (327 mg, 0.99 mmol). MS (m/z, MH+): 330.2
WORKUP
后处理
- temperaturethe reaction mixture was refluxed for 48 h
- filtrationThe inorganic precipitate was filtered off
- washwashed with ethyl acetate
- customthe solvent of the mother liquor was evaporated in vacuo
- customThe residue was purified by column chromatography (ethyl acetate/heptanes)