Hydrochloric Acid → {2-[2-(Hydroxyimino-phenyl-methyl)-phenyldisulfanyl]-phenyl}-phenyl-methanone

HRID 1378835

반응식

HRID 1378835 반응식
[C:1]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[S:15][S:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[C:23]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:24])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:32][OH:33].Cl.C(OCC)(=O)C>C(O)C.N1C=CC=CC=1>[OH:33][N:32]=[C:1]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[S:15][S:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[C:23]([C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)=[O:24]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 443297Hydroxyamine hydrochlorideHCID 18935315[2-(2-Benzoyl-phenyldisulfanyl)-phenyl]-phenylmethanone

생성물 1

HCID 6483564{2-[2-(Hydroxyimino-phenyl-methyl)-phenyldisulfanyl]-phenyl}-phenyl-methanone수율 35.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 1049Pyridine용매

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.;

후처리

  1. temperaturethe solution was refluxed for 90 minutes
  2. temperatureThe solution was cooled
  3. customthe layers were separated
  4. washthe organic portion was washed with brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated to dryness
  8. customthe residue was triturated with 75% hexane/25% ethyl acetate

출처 및 근거

ORD 기록
ord-c3a96cf56fd54e0bbbaa3306347886dd
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05668291

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