Ethanol → N-(3-methyl-benzylidene)-N'-(7-morpholin-4-yl-3-phenyl-pyrazolo[1,5-a]pyrimidin-5-yl)-hydrazine
반응식
Cl[C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[N:5]2[N:14]=[CH:15][C:16]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[C:4]2[N:3]=1.O.[NH2:24][NH2:25].[CH2:26](O)[CH3:27]>>[CH3:19][C:18]1[CH:17]=[C:16]([CH:4]=[CH:26][CH:27]=1)[CH:15]=[N:24][NH:25][C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[N:5]2[N:14]=[CH:15][C:16]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[C:4]2[N:3]=1참가 물질
반응 조건
- 온도
- 150 °C
실험 절차
There was suspended, in ethanol (2 mL), 5-chloro-7-morpholin-4-yl-3-phenyl-pyrazolo[1,5-a]pyrimidine (42.1 mg, 0.134 mM) and then hydrazine monohydrate (65.0 μL, 1.34 mM) was added to the suspension. This suspension was stirred at 150° C. for 20 minutes under the irradiation with microwaves, the solvent was then distilled off, the resulting residue was diluted with a saturated aqueous common salt solution and extracted with ethyl acetate. The extracts thus obtained were combined, dried over anhydrous sodium sulfate, and the solvent was then distilled off. The resulting residue was suspended in ethanol (2 mL), then acetic acid (2.0 μL, 0.035 mM) and 3-methyl-benzaldehyde (15.8 μL, 0.134 mM) were added to the suspension and the mixture was stirred at room temperature for 2 hours and a half.
후처리
- distillationthe solvent was then distilled off
- additionthe resulting residue was diluted with a saturated aqueous common salt solution
- extractionextracted with ethyl acetate
- customThe extracts thus obtained
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was then distilled off
- additionacetic acid (2.0 μL, 0.035 mM) and 3-methyl-benzaldehyde (15.8 μL, 0.134 mM) were added to the suspension
- stirringthe mixture was stirred at room temperature for 2 hours
출처 및 근거
- ORD 기록
- ord-45991ac0a9554cacb441d19bbeeec47b
- 출처 데이터셋
- uspto-grants-2012_11
- 특허 번호
- US08314098B2
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