HRID1962987

反应详情

EQUATION

反应方程式

HRID 1962987 的结构方程式

PROCEDURE

实验过程

A solution of 5-[3-(4-fluoro-phenyl)-5-((E)-styryl)-isoxazol-4-ylmethoxy]-pyridine-2-carboxylic acid ethyl ester (1.2 g, 3.24 mmol) in methanol (60 mL) was treated at room temperature with sodium borohydride (255.4 mg, 6.48 mmol) and stirred for 1 h. After quenching with aqueous citric acid (100 mL of a 10% solution) and extraction with ethyl acetate the organic phase was dried over sodium sulfate, filtered and concentrated. Purification by chromatography (silica, heptane:ethyl acetete=1:1 to 0:1) afforded the title compound as a white solid (710 mg, 59%). MS: m/e=373.2 [M+H]+.

WORKUP

后处理

  1. customAfter quenching with aqueous citric acid (100 mL of a 10% solution) and
  2. extractionextraction with ethyl acetate the organic phase
  3. dry with materialwas dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by chromatography (silica, heptane:ethyl acetete=1:1 to 0:1)