HRID84471

反应详情

EQUATION

反应方程式

HRID 84471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 4,5-dihydrobenzo[b]thieno[2,3-d]oxepine (440 mg, 2.2 mmol) and acetic acid (10 ml) in dichloromethane (10 ml) at 0° C., was added N-bromosuccinimide in portions. Reaction mixture was stirred for 18 hours, allowing solution to raise to room temperature before being concentrated in-vacuo. Residue was dissolved in ethyl acetate and sat. sodium carbonate solution. Organic phase was washed with water and brine, dried (Na2SO4) and concentrated in-vacuo to give 2-bromo-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine.

WORKUP

后处理

  1. customReaction mixture
  2. concentrationbefore being concentrated in-vacuo
  3. dissolutionResidue was dissolved in ethyl acetate
  4. washOrganic phase was washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in-vacuo