HRID1197860
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas cooled
- custompartitioned between water (30 ml) and dichloromethane (45 ml)
- customThe dichloromethane layer was separated
- customdried
- concentrationconcentrated under reduced pressure
- customto give an oil