HRID359454

反应详情

EQUATION

反应方程式

HRID 359454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the product of stage (i) (280 mg) in a mixture of ethanol (40 ml), 2N hydrochloric acid (0.7 ml) and water (5 ml; added to dissolve some precipitated hydrochloride of the starting material) was hydrogenated at room temperature and atmospheric pressure, using 10% palladium on carbon (50% w/w with H2O, 330 mg) as the catalyst. After 1 h; when 22 ml (0.92 mmol) of hydrogen had been absorbed, the reaction was stopped. The mixture was filtered and the filtrate was evaporated to give a foam (302 mg). The foam was crystallised from ethanol (ca. 3 ml) to give the title compound (196 mg) as a powder, with m.p. 229°-232°.

WORKUP

后处理

  1. additionadded
  2. customwas hydrogenated at room temperature
  3. filtrationThe mixture was filtered
  4. customthe filtrate was evaporated