HRID342423

反应详情

EQUATION

反应方程式

HRID 342423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-methyl-7-nitrobenzo[b]furan (1.77 g) and aluminum chloride (2.66 g) in dichloromethane (40 ml) was added dropwise a solution of dichloromethyl methyl ether (3.6 ml) in dichloromethane (10 ml). The mixture was stirred at ambient temperature for 30 minutes and the reaction mixture was poured into a mixture of ice and 1N-hydrochloric acid. The separated oil was extracted with dichloromethane and the extract was washed with brine, aqueous saturated sodium bicarbonate and brine. Then, the solution was dried over sodium sulfate and evaporated in vacuo. The obtained oil was crystallized from diethyl ether to give 3-formyl-2-methyl-7-nitrobenzo[b]furan (1.83 g).

WORKUP

后处理

  1. extractionThe separated oil was extracted with dichloromethane
  2. washthe extract was washed with brine, aqueous saturated sodium bicarbonate and brine
  3. dry with materialThen, the solution was dried over sodium sulfate
  4. customevaporated in vacuo
  5. customThe obtained oil was crystallized from diethyl ether