반응 #1471085

반응 방정식

4-[4-[2-(N-dodecyl-N-methylamino)ethoxy]-2-methoxyphenyl]-1,1,1-trifluoro-2-butanone

hydrobromic acid

→

title compound

수율 40.0%

7-[2-(N-Dodecyl-N-methylamino)ethoxy]-3,4dihydro-2-(trifluoromethyl)-2H-1-benzopyran-2-ol

수율 40.0%

용매

water

반응 조건

후처리

1. 1
   온도was refluxed for 3.5 h
2. 2
   추출extracted with dichloromethane
3. 3
   세척The organic layer was washed with sat. sodium bicarbonate, brine
4. 4
   건조dried over magnesium sulfate
5. 5
   농축concentrated in vacuo
6. 6
   기타The residue was chromatographed on silica gel (ethyl acetate/acetone 3:1)

실험 절차

A mixture of 4-[4-[2-(N-dodecyl-N-methylamino)ethoxy]-2-methoxyphenyl]-1,1,1-trifluoro-2-butanone (157 mg, 0.33 mmol) and hydrobromic acid (47%, 3 ml) was refluxed for 3.5 h. After cooling to r.t., the mixture was diluted with water, extracted with dichloromethane. The organic layer was washed with sat. sodium bicarbonate, brine, dried over magnesium sulfate and concentrated in vacuo. The residue was chromatographed on silica gel (ethyl acetate/acetone 3:1) to afford the title compound (60 mg, 40%) as a clear oil.

출처