反应详情

39.6 Parts of 1-(4-fluorophenyl)-1,3-dihydro-1-[3-(tetrahydro-2H-pyran-2-yloxy)propyl]isobenzofuran were dissolved in 9.8 parts of a hydrochloric acid solution 0.1M and 788 parts of ethanol and the whole was stirred and refluxed for 1 hour. The solvent was evaporated and the residue was taken up in methylbenzene and water. The organic phase was separated, washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (99:1 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 24.2 parts of 1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-1-propanol as a residue (intermediate 94).

1. temperaturerefluxed for 1 hour
2. customThe solvent was evaporated
3. customThe organic phase was separated
4. washwashed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (99:1 by volume) as eluent
10. customThe pure fractions were collected
11. customthe eluent was evaporated