반응 #63589

반응 방정식

α-(3-bromopropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetyl chloride

ethanol

→

ethyl α-(3-bromopropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetate

용매

methylbenzene

반응 조건

후처리

1. 1
   기타The reaction mixture was evaporated
2. 2
   기타the latter was evaporated again
3. 3
   세척The whole was washed with a saturate sodium hydrogen carbonate solution and with water
4. 4
   기타dried
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The residue was purified by column-chromatography over silica gel using
8. 8
   workup.ADDITIONa mixture of trichloromethane and hexane (50:50 by volume) as eluent
9. 9
   기타The pure fractions were collected
10. 10
    기타the eluent was evaporated

실험 절차

A mixture of 30 parts of α-(3-bromopropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetyl chloride, 9.3 parts of ethanol and 90 parts of methylbenzene was stirred overnight at room temperature. The reaction mixture was evaporated, the residue was taken up in ethanol and the latter was evaporated again. The residue was taken up in 2,2'-oxybispropane. The whole was washed with a saturate sodium hydrogen carbonate solution and with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and hexane (50:50 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 19.6 parts of ethyl α-(3-bromopropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetate as a residue (intermediate 18).

출처