Hydrochloric Acid → 4,7-dihydro-1,6-dimethyl-3-phenyl-4-(2-methylphenyl)-1H-pyrazolo[3,4-b]pyridin-5-carboxylic acid ethyl ester, hydrochloride

HRID 1031525

반응식

HRID 1031525 반응식
[CH2:1]([O:3][C:4](=[O:17])[C:5](=[CH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH3:16])[C:6]([CH3:8])=O)[CH3:2].[CH3:18][N:19]1[C:23]([NH2:24])=[CH:22][C:21]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[N:20]1.[ClH:31].CO>C(O)C>[ClH:31].[CH2:1]([O:3][C:4]([C:5]1[CH:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])[C:22]2[C:21]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)=[N:20][N:19]([CH3:18])[C:23]=2[NH:24][C:6]=1[CH3:8])=[O:17])[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 5177791-Methyl-3-phenyl-1H-pyrazol-5-amineHCID 54239661Ethyl-2-(2-methylbenzyliden)acetoacetate2회

생성물 1

HCID 1372254604,7-dihydro-1,6-dimethyl-3-phenyl-4-(2-methylphenyl)-1H-pyrazolo[3,4-b]pyridin-5-carboxylic acid ethyl ester, hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl-2-(2-methylbenzyliden)acetoacetate (0.050 mol) is added to 1-methyl-3-phenyl-5-pyrazolamine (0.050 mol) in ethanol (50 ml) and refluxed for 90 minutes. The mixture is then cooled to room temperature, further ethyl-2-(2-methylbenzyliden)acetoacetate (0.050 mol) is added thereto, and the mixture refluxed for further 90 minutes. The reaction mixture is then cooled, the solvent is evaporated, and the residue is taken up in ethyl ether, collected by filtration, and dried. The product is dissolved in methanol and a mixture of hydrochloric acid and methanol (45 mmol of HCl) is added thereto. The product of the title precipitates by adding ethyl ether. M.p. 187° C. (dec.).

후처리

  1. temperaturerefluxed for 90 minutes
  2. temperaturethe mixture refluxed for further 90 minutes
  3. temperatureThe reaction mixture is then cooled
  4. customthe solvent is evaporated
  5. filtrationcollected by filtration
  6. customdried
  7. dissolutionThe product is dissolved in methanol
  8. additionis added
  9. customThe product of the title precipitates
  10. additionby adding ethyl ether

출처 및 근거

ORD 기록
ord-a78c6a8330e642d08d1e3b3b76774091
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04954508

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