HRID1164160

反应详情

EQUATION

反应方程式

HRID 1164160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 98 mg of (13E)-(6RS,9α,11α,15S)-6,9-epithio-11,15-dihydroxyprost-13-enoic acid (prepared as described in Example 2) and 52 μl of triethylamine in 3 ml of acetone was added 49 μl of isobutyl chloroformate at 0° C., and the mixture was stirred at 0° C. for 30 minutes. To it were added 1.4 ml of pyridine and 202 mg of 4-hydroxybenzaldehyde semicarbazone at ambient temperature, and the mixture was stirred at room temperature for 5 hours. The reaction mixture was concentrated under reduced pressure. The residue was purified by recrystallization from acetonitrile to give 29.5 mg of the title compound having the following physical characteristics: melting point: 90°-91° C.;

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 5 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customThe residue was purified by recrystallization from acetonitrile