HRID1631882

反应详情

EQUATION

反应方程式

HRID 1631882 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-(4-bromo-2,6-dimethyl-phenyl)-5-(cyclohexyl-hydroxy-methyl)-3-methoxy-cyclopent-2-enone (1.38 g, 3.4 mmol) in ethanol (27.6 ml) and 2N aqueous hydrochloric acid (13.8 ml) is subjected to microwave irradiation at 130° C. for 40 minutes. The reaction mixture is concentrated under vacuum to remove ethanol. The aqueous layer was extracted with ethyl acetate (3×100 ml) and combined organic layers are dried with sodium sulfate and concentrated under vacuum to obtain crude mass. The compound was purified by column chromatography to give 2-(4-bromo-2,6-dimethyl-phenyl)-4-[1-cyclohexyl-meth-(E)-ylidene]-cyclopentane-1,3-dione (250 mg).

WORKUP

后处理

  1. customirradiation at 130° C. for 40 minutes
  2. concentrationThe reaction mixture is concentrated under vacuum
  3. customto remove ethanol
  4. extractionThe aqueous layer was extracted with ethyl acetate (3×100 ml)
  5. dry with materialare dried with sodium sulfate
  6. concentrationconcentrated under vacuum
  7. customto obtain crude mass
  8. customThe compound was purified by column chromatography