Hydrochloric Acid → Acetamide, N-(3-bromophenyl)-2-(hydroxyimino)-

HRID 2284389노트

반응식

HRID 2284389 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Cl[C:10](Cl)(Cl)[CH:11]([OH:13])O.Cl.[NH2:17][OH:18].S([O-])([O-])(=O)=O.[Na+].[Na+].Cl>O>[Br:1][C:2]1[CH:3]=[C:4]([NH:5][C:11](=[O:13])[CH:10]=[N:17][OH:18])[CH:6]=[CH:7][CH:8]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 115623-BromoanilineHCID 24436Sodium SulfateHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 6739944Acetamide, N-(3-bromophenyl)-2-(hydroxyimino)-수율 85%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

To a 3000 mL round bottom flask, 3-bromoaniline (50 g, 0.2907 mol), water (1500 mL), chloral hydrate (57.7 g, 0.3488 mol), hydroxylamine hydrochloride (64.6 g, 0.9302 mol) and sodium sulphate (250 g) were added. To this reaction mixture was slowly added concentrated HCl (76 mL). The reaction mixture was stirred at 90° C. for 2 hours. The white precipitate was formed and was collected by filtration. The white solid was dried to provide the title compound [60 g, 85%]. 1H NMR (300 MHz, DMSO-d6): δ 12.28 (s, 1H), 10.38 (s, 1H), 8.03 (t, J=1.5 Hz, 1H), 7.62-7.65 (m, 2H), 7.29-7.31 (m, 2H). LC-MS (ESI): Calculated mass: 242.0; Observed mass [M+H]+: 243.0 (RT: 0.17 min).

후처리

  1. customThe white precipitate was formed
  2. filtrationwas collected by filtration
  3. customThe white solid was dried

출처 및 근거

ORD 기록
ord-0cfd40d6645c485fb4aa9b15bbd9fdcf
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145411B2

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