HRID1164158

反应详情

EQUATION

反应方程式

HRID 1164158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 70 mg of (13E)-(6RS,9α,11α,15S)-6,9-epithio-11,15-dihydroxyprost-13-enoic acid (prepared as described in Example 2), 3 ml of tetrahydrofuran and 34.5 μl of triethylamine was stirred at room temperature for 5 minutes, and then stirred with 27.7 μl of pivaloyl chloride. To the mixture were added 70 μl of triethylamine and 0.5 ml of 2-hydroxyethanol, and the mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate, washed with water, and a saturated aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using a mixture of ethyl acetate and cyclohexane (2:1) as eluent to give 92 mg of the title compound having the following physical characteristics:

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 18 hours
  2. washwashed with water
  3. dry with materiala saturated aqueous solution of sodium chloride, dried over magnesium sulphate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel using
  6. additiona mixture of ethyl acetate and cyclohexane (2:1) as eluent