HRID456588

反应详情

EQUATION

反应方程式

HRID 456588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,4-benzodioxanecarboxaldehyde [RN 29668-44-8](1.5 g, 9.14 mmol), trimethylsulfonium methyl sulfate (2.24 g, 11.9 mmol), dichloromethane (35 ml) and 50% aqueous sodium hydroxide (5 ml) were vigorously stirred for 70 hours. The mixture was partitioned between water and diethyl ether and the layers separated. The aqueous phase was extracted with diethyl ether. The combined organic phases were washed with water, brine, then dried over magnesium sulfate and evaporated to give crude 6-oxiranyl-2,3-dihydro-benzo[1,4]dioxine (1.64 g, 100%).

WORKUP

后处理

  1. customThe mixture was partitioned between water and diethyl ether
  2. customthe layers separated
  3. extractionThe aqueous phase was extracted with diethyl ether
  4. washThe combined organic phases were washed with water, brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated