تفاعل #1960488

معادلة التفاعل

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

المذيبات

N,N-diethylaniline

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   استخلاصThe batch is extracted with MTBE
3. 3
   غسيلthe organic phase is washed with saturated sodium chloride solution
4. 4
   أخرىThe solution is dried
5. 5
   أخرىevaporated to dryness
6. 6
   أخرىThe crude product is purified by column chromatography (SiO2, 1-chlorobutane)

الإجراء التجريبي

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.

المصدر