反应 #2566

反应方程式

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-tetrahydropyranyloxymethyl-N-(2-methoxyphenyl)benzene sulfonamide

p-toluenesulfonic acid monohydrate

sodium bicarbonate

→

title compound

收率 100.1%

N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-4-hydroxymethyl-N-(2-methoxyphenyl)benzene sulfonamide

收率 100.1%

溶剂

methanol

methanol

反应条件

后处理

1. 1
   其他at room temperature
2. 2
   其他was removed by evaporation
3. 3
   其他the resulting reaction solution
4. 4
   萃取extracted with ethyl acetate
5. 5
   洗涤washed with water and saturated brine
6. 6
   萃取The water layer was extracted with ethyl acetate
7. 7
   洗涤washed with water and saturated brine
8. 8
   干燥dried on anhydrous sodium sulfate
9. 9
   其他Thereafter, the solvent was removed by evaporation
10. 10
    其他the resulting residue was purified by a silica gel column chromatography (ethyl acetate)

实验过程

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-tetrahydropyranyloxymethyl-N-(2-methoxyphenyl)benzene sulfonamide (101 mg, 0.165 mmol) was dissolved in methanol (5 ml) to which was subsequently added p-toluenesulfonic acid monohydrate (35 mg, 0.18 mmol) at room temperature. After 2 hour of stirring at the same temperature, methanol was removed by evaporation, and the resulting reaction solution was mixed with saturated sodium bicarbonate aqueous solution (5 ml), extracted with ethyl acetate, and washed with water and saturated brine. The water layer was extracted with ethyl acetate, and washed with water and saturated brine, and the organic layers were combined and dried on anhydrous sodium sulfate. Thereafter, the solvent was removed by evaporation, and the resulting residue was purified by a silica gel column chromatography (ethyl acetate) to obtain 87 mg (100%) of the title compound in the form of colorless oil.

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