反应详情

To 1190 parts of 1,1'-oxybisethane were added at once 50 parts of lithium aluminium hydride. Then there was added dropwise a solution of 213.7 parts of 2-(4-fluorobenzoyl)benzoic acid in 875 parts of 1,1'-oxybixethane so that the mixture was kept at reflux temperature. Upon completion, stirring was continued first for 30 minutes at room temperature, then for 2 hours at reflux and further overnight at room temperature. The reaction mixture was cooled to 0° C. and there were added dropwise successively 50 parts of water, 50 parts of a 15% sodium hydroxide solution and 150 parts of water all at 0° C. The reaction mixture was filtered over Hyflo and washed thoroughly with 1,1'-oxybisethane. The organic phase was separated, washed with water, dried, filtered and evaporated. The residue was crystallized from a mixture of benzene and hexane, yielding 170.4 parts of α-(4-fluorophenyl)-1,2-benzenedimethanol; mp. ±75° C. (intermediate 91).

1. temperatureat reflux temperature
2. temperatureThe reaction mixture was cooled to 0° C.
3. filtrationThe reaction mixture was filtered over Hyflo
4. washwashed thoroughly with 1,1'-oxybisethane
5. customThe organic phase was separated
6. washwashed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe residue was crystallized from a mixture of benzene and hexane