HRID37423

反应详情

EQUATION

反应方程式

HRID 37423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.55 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodioxepine (see Example 10) were dissolved in 70 ml of methylene chloride (CH2Cl2) and treated at 0° C. under an Argon atmosphere with a solution of 8.0 g of Br2 in 30 ml of CH2Cl2. The mixture was warmed to room temperature and left to react for 1 hour. It was then poured on to ice and extracted with ether. Washing with NaHCO3 solution and water, drying and evaporation yielded 13.35 g of 7-bromo-3,4-dihydro-3,3-dimethyl-2H-1,5-benzodioxepine as a colorless oil which was 94.5% pure and which contained 4.7% of starting material; it was processed in the crude state.

WORKUP

后处理

  1. waitleft
  2. customto react for 1 hour
  3. additionIt was then poured on to ice
  4. extractionextracted with ether
  5. washWashing with NaHCO3 solution and water
  6. customdrying
  7. customevaporation