HRID4428

反应详情

EQUATION

反应方程式

HRID 4428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

21.5 g (0.15 mole) of 1-chloroethylchloroformate are added in a single portion to a solution of 2,3-dihydro-2,2-dimethyl-7-benzofuranol (24.6 g; 0.15 mole) in dichloromethane (150 ml). The mixture is cooled to between 0° and 5° C., and 12 g (0.15 mole) of pyridine are added dropwise. The mixture is stirred for 3 hours at 20° C. The organic phase is then washed with 2×50 ml of iced water. It is dried over magnesium sulphate and the solvent is evaporated. A yellow oil is obtained which is distilled. 34.1 g of the expected carbonate is then recovered (84% yield).

WORKUP

后处理

  1. temperatureThe mixture is cooled to between 0° and 5° C.
  2. washThe organic phase is then washed with 2×50 ml of iced water
  3. dry with materialIt is dried over magnesium sulphate
  4. customthe solvent is evaporated
  5. customA yellow oil is obtained which
  6. distillationis distilled
  7. custom34.1 g of the expected carbonate is then recovered (84% yield)