反应详情

To a stirred mixture of 11 parts of (-)-(R)-3-(4-fluorophenoxy)-1,2-propanediol, 23.3 parts of pyridine and 240 parts of trichloromethane were added 12.3 parts of 4-methylbenzenesulfonyl chloride. The whole was stirred overnight at room temperature. It was washed successively with acid water, a sodium carbonate solution and water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 13.5 parts (67.2%) of (+)-(S)-3-(4-fluorophenoxy)-1,2-propanediol, O1 -4-methylbenzenesulfonate; [α]D =+11.11° (c=0.5% in trichloromethane) (147).

1. washIt was washed successively with acid water
2. dry with materiala sodium carbonate solution and water, dried
3. filtrationfiltered
4. customevaporated
5. customThe residue was purified by column chromatography over silica gel using
6. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
7. customThe pure fractions were collected
8. customthe eluent was evaporated