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

HRID 3747

反応式

HRID 3747 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 1049Pyridine溶媒

実験手順

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.;

後処理

  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

出典と根拠

ORDレコード
ord-169cfd162f7a4903b732bbd90fedb229
出典データセット
uspto-grants-1998_03
特許番号
US05734081

関連ノート

読み込み中…