Ethanol → HCID 21847821, 화합물

HRID 618668노트

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HRID 618668 반응식
[N:1]1([C:6]2[CH:7]=[CH:8][C:9]([N+:14]([O-])=O)=[C:10]([CH:13]=2)[C:11]#[N:12])[CH:5]=[CH:4][N:3]=[CH:2]1.O.NN.C([OH:22])C>[Ni].CC(N(C)C)=O>[NH2:14][C:9]1[CH:8]=[CH:7][C:6]([N:1]2[CH:5]=[CH:4][N:3]=[CH:2]2)=[CH:13][C:10]=1[C:11]([NH2:12])=[O:22]

참가 물질

6

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 218478205-(1-Imidazolyl)-2-nitrobenzonitrile

생성물 1

HCID 21847821HCID 21847821, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 31374Dimethylacetamide용매

반응 조건

온도
40 °C

실험 절차

A mixture of 5-(1-imidazolyl)-2-nitrobenzonitrile (2.14 g), hydrazine hydrate (2 ml), ethanol (25 ml) and DMA (10 ml) was stirred and heated to 40° C. Raney nickel (0.6 g) was added in portions whilst maintaining the temperature at 40-50° C. The mixture was stirred at 40-50° C. for 2 hours. The Raney nickel was filtered off, the mixture was evaporated and the residue was triturated with ethyl acetate (10 ml) to give 2-amino-5-(1-imidazolyl)benzamide (2.03 g); NMR Spectrum: (CD3SOCD3) 6.70 (s, 2H), 6.79 (d, 1H), 7.03 (s, 1H), 7.2 (s, 1H), 7.37 (s, 1H), 7.55 (s, 1H), 7.71 (d, 1H), 7.73 (s, 1H), 8.02 (s, 1H);

후처리

  1. temperaturewhilst maintaining the temperature at 40-50° C
  2. stirringThe mixture was stirred at 40-50° C. for 2 hours
  3. filtrationThe Raney nickel was filtered off
  4. customthe mixture was evaporated
  5. customthe residue was triturated with ethyl acetate (10 ml)

출처 및 근거

ORD 기록
ord-2d40baf8efd54298af009eb1a0c30746
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05955464

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