HRID2220576

反应详情

EQUATION

反应方程式

HRID 2220576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

31.0 g (0.17 mol) of 1-butoxy-2,3-difluorobenzene are initially introduced in 200 ml of THF, and 100 ml (0.16 mol) of n-BuLi (15% soln. in hexane) are added at −70° C. After 2 h at this temperature, a solution of 35.6 g (0.16 mol) of 4′-propylbicyclohexyl-4-one in 200 ml of THF is metered in, and the batch is stirred for 2.5 h. The reaction mixture is hydrolysed with ice-cooling and acidified using 2 N HCl. The solution is extracted with MTBE, and the combined organic phases are washed with sat. sodium chloride solution and dried using sodium sulfate. The solution is concentrated to dryness, and the crude product (66.3 g of yellow solid) is used directly for the following reaction.

WORKUP

后处理

  1. temperaturecooling
  2. extractionThe solution is extracted with MTBE
  3. washthe combined organic phases are washed with sat. sodium chloride solution
  4. customdried
  5. concentrationThe solution is concentrated to dryness
  6. customthe crude product (66.3 g of yellow solid) is used directly for the following reaction