反応 #1960496

反応方程式

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

→

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

溶媒

N,N-diethylaniline

MTBE

反応条件

後処理

1. 1
   洗浄washed a number of times with 3 N HCl
2. 2
   その他The organic phase is dried
3. 3
   その他evaporated to dryness
4. 4
   その他The residue is purified by column chromatography (SiO2, n-heptane:MTBE=4:1)

実験手順

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.

出典