反应详情

To a stirred mixture of 18.3 parts of 4-(4-fluoro-2-nitrophenoxy)cyclohexanol, 6.23 parts of pyridine and 135 parts of trichloromethane were added dropwise, during a 10 minutes period, 9 parts of methanesulfonyl chloride. Upon completion, stirring was continued overnight at room temperature. The whole was further stirred and refluxed for 2 hours. The reaction mixture was evaporated and the residue was stirred in water. The product was extracted with trichloromethane. The extract was 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. The residue was crystallized from 1,1'-oxybisethane, yielding 8.5 parts of 4-(4-fluoro-2-nitrophenoxy)cyclohexanol methanesulfonate (ester); mp. 111.7° C. (intermediate 102).

1. additionwere added dropwise, during a 10 minutes period
2. stirringThe whole was further stirred
3. temperaturerefluxed for 2 hours
4. customThe reaction mixture was evaporated
5. stirringthe residue was stirred in water
6. extractionThe product was extracted with trichloromethane
7. customThe extract was dried
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
13. customThe residue was crystallized from 1,1'-oxybisethane