反応 #2566

反応方程式

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

p-toluenesulfonic acid monohydrate

sodium bicarbonate

→

title compound

収率 100.1%

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

収率 100.1%

溶媒

methanol

methanol

反応条件

後処理

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

実験手順

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.

出典