反応 #63589

反応方程式

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

ethanol

→

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

溶媒

methylbenzene

反応条件

後処理

1. 1
   その他The reaction mixture was evaporated
2. 2
   その他the latter was evaporated again
3. 3
   洗浄The whole was washed with a saturate sodium hydrogen carbonate solution and with water
4. 4
   その他dried
5. 5
   ろ過filtered
6. 6
   その他evaporated
7. 7
   その他The 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
   その他The pure fractions were collected
10. 10
    その他the eluent was evaporated

実験手順

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).

出典