HRID2120693

反应详情

EQUATION

反应方程式

HRID 2120693 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A solution of the allylic alcohol 22-3 (0.26 g, 0.57 mmol) in (EtO)3CMe (10 mL) was treated with 100 μL of a 1 mL solution of (EtO)3CMe containing 10 μL of propionic acid. The yellow solution was heated at 150° C. for 90 minutes. The solution was cooled to room temperature and poured into 1N HCl/brine. The mixture was extracted with CHCl3, dried, concentrated, and purified on silica gel (90:5:5 CHCl3:EtOAc:MeOH) to give 0.143 g (48%)of 22-4.

WORKUP

后处理

  1. temperatureThe solution was cooled to room temperature
  2. extractionThe mixture was extracted with CHCl3
  3. customdried
  4. concentrationconcentrated
  5. custompurified on silica gel (90:5:5 CHCl3:EtOAc:MeOH)