HRID505545

反应详情

EQUATION

反应方程式

HRID 505545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Boron tribromide as a 1 M solution in dichloromethane (41 mL, 41 mmol) was added to 1-bromo-2,5-dichloro-3-methoxybenzene (10.5 g, 41 mmol) in dichloromethane (100 mL) at −78° C. under N2. The reaction mixture was allowed to warm to room temperature, and after 21 hours, the mixture was poured into 100 g of ice, diluted with 100 g of water, and the organic layer separated. The aqueous layer was extracted with dichloromethane (200 mL) and the combined organic extracts were dried (MgSO4), filtered and the solvent was evaporated under reduced pressure. 1H NMR (CDCl3) δ 7.20 (m, 1H), 7.00 (m, 1H), 5.70 (s, 1H).

WORKUP

后处理

  1. customthe organic layer separated
  2. extractionThe aqueous layer was extracted with dichloromethane (200 mL)
  3. dry with materialthe combined organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent was evaporated under reduced pressure