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

HRID 2092531ノート

反応式

HRID 2092531 の反応式
[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

参加物

7

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-7e7ecfcaede04ef2bfec735986014352
出典データセット
uspto-grants-2013_05
特許番号
US08440662B2

反応ノート

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