Potassium Carbonate → HCID 178513408, 화합물

HRID 1710099

반응식

HRID 1710099 반응식
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[K+].[K+].[NH:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]([C:19]#[N:20])=[N:11]1>C(O)C.CO>[CH:15]1[CH:14]=[C:13]2[C:12]([NH:11][NH:10][C:18]2=[CH:17][CH:16]=1)=[C:19]([N:2]=[O:3])[NH2:20]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 4375561H-Indazole-3-carbonitrileHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 178513408HCID 178513408, 화합물수율 36.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

Hydroxylamine hydrochloride (1.5 g) and potassium carbonate (3.83 g) were stirred together in absolute ethanol (100 ml) for 15 minutes. Indazole-3-carbonitrile (2 g) was added and the solution heated at reflux for 4 hours, cooled to room temperature and diluted with methanol (5 ml). The solution was filtered and the solvent evaporated. The residue was extracted with anhydrous ether, the extracts were dried over MgSO4, filtered and the solvent removed to afford a white solid, which was recrystallised from acetone/dichloromethane to afford the title compound (900 mg), m.p. 155°-158° C. δH (360 MHz, CDCl3) 6.46 (1H, brm, N-OH), 7.17 (1H, t, J=1 Hz, H-6), 7.41 (1H, t, J=2 Hz, H-5), 7.55 (1H, d, J=2 Hz, H-4), 8.03 (1H, t, J=2 Hz, H-7); m/z (M+ , 100%), 176 (100), 144 (80), 119 (25), 92 (15).

후처리

  1. temperaturethe solution heated
  2. temperatureat reflux for 4 hours
  3. filtrationThe solution was filtered
  4. customthe solvent evaporated
  5. extractionThe residue was extracted with anhydrous ether
  6. dry with materialthe extracts were dried over MgSO4
  7. filtrationfiltered
  8. customthe solvent removed
  9. customto afford a white solid, which
  10. customwas recrystallised from acetone/dichloromethane

출처 및 근거

ORD 기록
ord-53e1ec03f4654b81a1784050e8a75879
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04952587

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