HRID713410

反应详情

EQUATION

反应方程式

HRID 713410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction mixture was refluxed for 48 h
  2. filtrationThe inorganic precipitate was filtered off
  3. washwashed with ethyl acetate
  4. customthe solvent of the mother liquor was evaporated in vacuo
  5. customThe residue was purified by column chromatography (ethyl acetate/heptanes)