반응 #2568

반응 방정식

water

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-formyl-N-(2-methoxyphenyl)benzenesulfonamide

hydroxyamine hydrochloride

sodium carbonate

→

title compound

수율 102.7%

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-(N-hydroxyimino)-N-(2-methoxyphenyl)benzenesulfonamide

수율 102.7%

용매

ethanol

반응 조건

후처리

1. 1
   기타ethanol was removed by evaporation
2. 2
   workup.ADDITIONthe resulting residue was mixed with water (10 ml)
3. 3
   기타to collect crystals
4. 4
   여과by filtration
5. 5
   세척The thus collected crystals were washed with water and hexane
6. 6
   workup.DISSOLUTIONdissolved in methylene chloride (50 ml)
7. 7
   건조dried on anhydrous sodium carbonate
8. 8
   기타Thereafter, the solvent was removed by evaporation

실험 절차

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-formyl-N-(2-methoxyphenyl)benzenesulfonamide (63 mg, 0.12 mmol) and hydroxyamine hydrochloride (9.5 mg, 0.132 mmol) were dissolved in ethanol (2 ml) to which were subsequently added anhydrous sodium carbonate (14 mg, 0.132 mmol) and water (1 ml). After 1.5 hours of stirring at room temperature, ethanol was removed by evaporation, and the resulting residue was mixed with water (10 ml) to collect crystals by filtration. The thus collected crystals were washed with water and hexane, dissolved in methylene chloride (50 ml) and then dried on anhydrous sodium carbonate. Thereafter, the solvent was removed by evaporation to obtain 65 mg (100%) of the title compound in the form of colorless powder.

출처