반응 #1960496

반응 방정식

6-(1-ethynylbutoxy)-7,8-difluoro-2-pentylchroman

→

5,6-difluoro-3-pentyl-8-propyl-1,2,3,8-tetrahydropyrano[3,2-f]-chromene

용매

N,N-diethylaniline

MTBE

반응 조건

후처리

1. 1
   세척washed a number of times with 3 N HCl
2. 2
   기타The organic phase is dried
3. 3
   기타evaporated to dryness
4. 4
   기타The residue is purified by column chromatography (SiO2, n-heptane:MTBE=4:1)

실험 절차

9.0 g (26.8 mmol) of 6-(1-ethynylbutoxy)-7,8-difluoro-2-pentylchroman are heated at 205° C. for 3 h in 90 ml of N,N-diethylaniline. The batch is diluted with MTBE and washed a number of times with 3 N HCl. The organic phase is dried using sodium sulfate and evaporated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:MTBE=4:1), giving 5,6-difluoro-3-pentyl-8-propyl-1,2,3,8-tetrahydropyrano[3,2-f]-chromene as a pale-brown oil.

출처