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

HRID 2092531노트

반응식

HRID 2092531 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 sulfate (250 g) were added. To this reaction mixture conc. HCl (76 mL) was slowly added. The reaction mixture was stirred at 90° C. for 2 h. The white precipitate was formed and was collected by filtration. The white solid was dried to get 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: 243.0 [M+H]+ (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-7e7ecfcaede04ef2bfec735986014352
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08440662B2

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