Hydroxylamine → HCID 178448432, 화합물

HRID 1966762노트

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HRID 1966762 반응식
[Br:1][C:2]1[CH:22]=[CH:21][C:5]2[N:6]([C:17]([CH3:20])([CH3:19])[CH3:18])[C:7]([C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11]#[N:12])=[N:8][C:4]=2[CH:3]=1.[NH2:23][OH:24]>CCO>[Br:1][C:2]1[CH:22]=[CH:21][C:5]2[N:6]([C:17]([CH3:18])([CH3:19])[CH3:20])[C:7]([C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11]([NH:23][OH:24])=[NH:12])=[N:8][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 58542011HCID 58542011, 화합물

생성물 1

HCID 178448432HCID 178448432, 화합물수율 81%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

To a suspension of 2-(5-bromo-1-tert-butyl-1H-benzimidazol-2-yl)-benzonitrile (765 mg, 2.16 mmol) in EtOH (15 mL) is added hydroxylamine 50% aqueous solution (2.85 mL, 43.19 mmol) at room temperature. The solution is heated to 80° C. for 2 hours. The reaction mixture is cooled to room temperature and the ethanol removed in vacuo. Water (30 mL) is added to the reaction mixture and the resultant precipitate is filtered and washed with 10% EtOAc/heptane (10 mL) to afford 2-(5-bromo-1-tert-butyl-1H-benzimidazol-2-yl)-N-hydroxy-benzamidine (716 mg, 81%).

후처리

  1. temperatureThe reaction mixture is cooled to room temperature
  2. customthe ethanol removed in vacuo
  3. additionWater (30 mL) is added to the reaction mixture
  4. filtrationthe resultant precipitate is filtered
  5. washwashed with 10% EtOAc/heptane (10 mL)

출처 및 근거

ORD 기록
ord-8631b78c487a43aaa55115e2ec4e8469
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08420655B2

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