HRID222481

反应详情

EQUATION

反应方程式

HRID 222481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methacryloyl chloride (50 ml, 0.5 mol) was added to suspension of 133.5 r AlCl3 (1 mol) in 500 ml CH2Cl2 at −78° C., stirred 20 min. Then indane (59 g, 0.5 mol) was added at the same temperature, allowed to warm to room temperature and then was stirred overnight. Next day the mixture obtained was poured carefully into mixture of ice (1000 g) and HCl (200 ml). The organic phase was separated, washed by water, 5% NaHCO3, and dried over MgSO4. Solvent was evaporated and residue was distilled in vacuum given 77.6 of product (83%), b.p. 118-120° C./0.5 torr.

WORKUP

后处理

  1. stirringwas stirred overnight
  2. customNext day the mixture obtained
  3. customThe organic phase was separated
  4. washwashed by water, 5% NaHCO3
  5. dry with materialdried over MgSO4
  6. customSolvent was evaporated
  7. distillationresidue was distilled in vacuum