반응 #3843

반응 방정식

Ethyl acetate

[2-(2-benzoyl-phenyldisulfanyl)-phenyl]phenyl-methanone

Hydroxylamine hydrochloride

HCl

→

title compound

수율 35.9%

{2-[2-(hydroxyimino-phenyl-methyl)-phenyldisulfanyl]phenyl}-phenyl-methanon

수율 35.9%

용매

ethanol

pyridine

반응 조건

후처리

1. 1
   온도the solution was refluxed for 90 minutes
2. 2
   온도The solution was cooled
3. 3
   기타the layers were separated
4. 4
   세척the organic portion was washed with brine
5. 5
   건조dried (MgSO4)
6. 6
   여과filtered
7. 7
   농축The filtrate was concentrated to dryness
8. 8
   기타the residue was triturated with 75% hexane/25% ethyl acetate

실험 절차

The [2-(2-benzoyl-phenyldisulfanyl)-phenyl]phenyl-methanone (0.55 g, 1.2 mmol) was diluted with ethanol (5 mL) and anhydrous pyridine (5 mL). Hydroxylamine hydrochloride (1 g, 14 mmol) was added and the solution was refluxed for 90 minutes. The solution was cooled and poured into cold aqueous HCl (1N). Ethyl acetate was added, the layers were separated, and the organic portion was washed with brine, dried (MgSO4), and filtered. The filtrate was concentrated to dryness and the residue was triturated with 75% hexane/25% ethyl acetate to give the title compound (0.19 g, 32%) as a white solid, mp 191°-193° C.;

출처