反应 #1960488

反应方程式

hydrochloric acid

7,8-difluoro-6-[1-(4-propylcyclohexyl)prop-2-ynyloxy]-chroman

potassium fluoride

water

→

5,6-difluoro-8-(4-propylcyclohexyl)-1,2,3,8-tetrahydropyrano[3,2-f]chromene

溶剂

N,N-diethylaniline

反应条件

后处理

1. 1
   温度After cooling
2. 2
   萃取The batch is extracted with MTBE
3. 3
   洗涤the organic phase is washed with saturated sodium chloride solution
4. 4
   其他The solution is dried
5. 5
   其他evaporated to dryness
6. 6
   其他The crude product is purified by column chromatography (SiO2, 1-chlorobutane)

实验过程

6.0 g (17.2 mmol) of 7,8-difluoro-6-[1-(4-propylcyclohexyl)prop-2-ynyloxy]-chroman are heated at 200° C. for 6 h together with 2.0 g (34.4 mmol) of potassium fluoride in 55 ml of N,N-diethylaniline. After cooling, water is added, and the mixture is acidified using 25% hydrochloric acid. The batch is extracted with MTBE, and the organic phase is washed with saturated sodium chloride solution. The solution is dried using sodium sulfate and evaporated to dryness. The crude product is purified by column chromatography (SiO2, 1-chlorobutane), giving 5,6-difluoro-8-(4-propylcyclohexyl)-1,2,3,8-tetrahydropyrano[3,2-f]chromene as a pale-brown oil.

来源