HRID1461283

反应详情

EQUATION

反应方程式

HRID 1461283 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The crude product of Step 5 (10.8 g, 40.0 mmol) was heated under reflux in toluene (100 m) for 30 min, cooled to room temperature, and extracted with 1N-HCl (3×50 ml). The extracts were basified with 10N-NaOH and extracted with dichloromethane (3×200 ml). The organic extracts were dried (MgSO4) and evaporated in vacuo to give an oil which was purified by chromatography (alumina; ether) to give the product (5.5 g, 95%) as an oil.

WORKUP

后处理

  1. extractionextracted with 1N-HCl (3×50 ml)
  2. extractionextracted with dichloromethane (3×200 ml)
  3. dry with materialThe organic extracts were dried (MgSO4)
  4. customevaporated in vacuo
  5. customto give an oil which
  6. customwas purified by chromatography (alumina; ether)