HRID1989946

反应详情

EQUATION

反应方程式

HRID 1989946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

10% Palladium on carbon (1.9 g, 50% wet) was added under argon to N-(1-ethyl-1H-pyrazol-3-yl)-3-{[(1S)-1-methyl-2-(methyloxy)ethyl]oxy}-5-[(phenylmethyl)oxy]benzamide (19.1 g, 46.7 mmol) in dry THF (100 mL) and ethanol (100 mL). The reaction mixture was degassed, placed under a hydrogen balloon and stirred for 16 hours. The mixture was filtered through diatomaceous earth and the filtrate was evaporated to give a brown oil. The residue was purified by column chromatography on silica, eluting with 40-65% ethyl acetate in hexanes, to give the desired product as a clear oil which crystallised on standing (11.35 g).

WORKUP

后处理

  1. customThe reaction mixture was degassed
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. customthe filtrate was evaporated
  4. customto give a brown oil
  5. customThe residue was purified by column chromatography on silica
  6. washeluting with 40-65% ethyl acetate in hexanes