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Water → 1H-Benzimidazole-4-carbohydrazide

HRID 1767681
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HRID 1767681 반응식
C[O:2][C:3]([C:5]1[C:10]2[N:11]=[CH:12][NH:13][C:9]=2[CH:8]=[CH:7][CH:6]=1)=O.O.[NH2:15][NH2:16].O>CCO>[N:11]1[C:10]2[C:5]([C:3]([NH:15][NH2:16])=[O:2])=[CH:6][CH:7]=[CH:8][C:9]=2[NH:13][CH:12]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 14970852methyl 1H-benzo[d]imidazole-4-carboxylate

생성물 1

HCID 450778831H-Benzimidazole-4-carbohydrazide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Benzimidazole ester 3 (1.65 g, 9.36 mmol), hydrazine monohydrate (10 mL), and water (3 mL) were refluxed in EtOH (60 mL) for 24 hs. Reaction mixture was cooled to room temperature and solid formed was filtered, washed with EtOH and dried to give 1.13 g (68%) of pure 4: 1H NMR (DMSO-d6) δ 12.31 (br.s, 1H), 10.59 (s, 1H), 8.44 (s, 1H), 7.86 (d, 1H, J=6.5 Hz), 7.76 (d, 1H, J=8.0 Hz), 7.34 (t, 1H, J=8.0 Hz), 4.68 (s, 2H).

후처리

  1. customReaction mixture
  2. customsolid formed
  3. filtrationwas filtered
  4. washwashed with EtOH
  5. customdried
  6. customto give 1.13 g (68%) of pure 4

출처 및 근거

ORD 기록
ord-6a4dd83572c947db8f9a9740f2244af9
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07235557B2

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