HRID582604

反应详情

EQUATION

反应方程式

HRID 582604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of 5.0 g (17 mmol) of 2-(2-hydroxy-3,3,3-trifluoropropyl)-6-nitro-3,4-dihydro-2H-1-benzopyran in a mixture of 60 ml of toluene and 20 ml of dichloromethane is stirred for 3 hours with 6.1 ml (52 mmol) of benzyl bromide, 0.55 g (1.7 mmol) of tetrabutylammonium bromide and a solution of 2.7 g (69 mmol) of sodium hydroxide in 5.4 ml of water. The reaction mixture is then diluted with dichloromethane and washed with water, then the organic phase is dried over sodium sulfate and concentrated under reduced pressure. By chromatography of the residue on a silica column using cyclohexane containing 0 to 50% of dichloromethane, 5.9 g of product are obtained.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialthe organic phase is dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customare obtained