HRID2364776

反应详情

EQUATION

反应方程式

HRID 2364776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of example 19A (1.017 g, 2.496 mmol) in ethanol (15 mL) and THF (15 mL) was added iron powder (0.836 g, 14.98 mmol) followed by ammonium chloride (0.401 g, 7.49 mmol) and water (3.75 mL). Reaction mixture was refluxed for 45 minutes. Slurry filtered through celite, washed with ethanol, combined filtrate was concentrated and the residue purified by column chromatography (gradient elution from 30% to 50% EtOAc:hexanes) to provide 1.09 g (77%) of the title compound.

WORKUP

后处理

  1. customReaction mixture
  2. temperaturewas refluxed for 45 minutes
  3. filtrationSlurry filtered through celite
  4. washwashed with ethanol
  5. concentrationwas concentrated
  6. customthe residue purified by column chromatography (gradient elution from 30% to 50% EtOAc:hexanes)