HRID1197860

反应详情

EQUATION

反应方程式

HRID 1197860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

The product of part (i) (3.2 g) was dissolved in acetic acid (25 ml) and diluted with 5N HCl (10 ml). After heating the mixture at 100° C. for 16 hours the mixture was cooled and partitioned between water (30 ml) and dichloromethane (45 ml). The dichloromethane layer was separated, dried and concentrated under reduced pressure to give an oil. The title compound was isolated by chromatography on silica gel using dichloromethane as the eluent. The product was characterised by 1H-NMR and mass spectrometry (yield=350 mg).

WORKUP

后处理

  1. temperaturewas cooled
  2. custompartitioned between water (30 ml) and dichloromethane (45 ml)
  3. customThe dichloromethane layer was separated
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customto give an oil