反应详情

To a stirred and cooled (ice-bath) mixture of 50 parts of fluorobenzene and 4.1 parts of 4-(4-fluorophenyl)-4-hydroxycyclohexanone were added portionwise 11 parts of aluminium chloride. Upon completion, stirring was continued for 2 hours while still cooling. The reaction mixture was decomposed by pouring onto a mixture of crushed ice and a hydrochloric acid solution. The product was extracted with methylbenzene. The extract was washed with water till neutralization, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated, yielding 4.3 parts (75.9%) of 4,4-bis(4-fluorophenyl)-1-cyclohexanone as a residue (intermediate 19).

1. temperaturecooled
2. stirringUpon completion, stirring
3. temperaturewhile still cooling
4. additionby pouring onto a mixture of crushed ice
5. extractionThe product was extracted with methylbenzene
6. washThe extract was washed with water till neutralization,
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified by column-chromatography over silica gel
11. customThe pure fractions were collected
12. customthe eluent was evaporated