Hydrochloric Acid → 6-(1-(azetidin-3-yl)piperidin-3-yl)-3-methyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one hydrochloride
반응식
[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([CH:12]3[CH2:17][CH2:16][CH2:15][N:14]([CH:18]4[CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19]4)[CH2:13]3)=[N:6][C:5]=2[N:4]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[N:3]=1.[ClH:35]>>[ClH:35].[NH:20]1[CH2:21][CH:18]([N:14]2[CH2:15][CH2:16][CH2:17][CH:12]([C:7]3[NH:8][C:9](=[O:11])[C:10]4[C:2]([CH3:1])=[N:3][N:4]([C:29]5[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=5)[C:5]=4[N:6]=3)[CH2:13]2)[CH2:19]1참가 물질
3
실험 절차
Into a 100-mL round-bottom flask, was placed a solution of tert-butyl 3-(3-(3-methyl-4-oxo-1-phenyl-4,5-dihydro-1H-pyrazolo[3,4-d]pyrimidin-6-yl)piperidin-1-yl)azetidine-1-carboxylate (200 mg, 0.43 mmol, 1.00 equiv) in hydrogen chloride (5 mL) at room temperature. The resulting solution was heated to reflux overnight. The resulting mixture was concentrated under vacuum. The resulting residue (150 mg) was purified by Prep-HPLC with the following conditions (Gilson Pre-HPLC): Column, SHISEIDO, CAPCELL PAK C18, 20 mm ID*250 mm, 5 u; mobile phase, methanol/H2O; Detector, UV 254 nm to yield 6-(1-(azetidin-3-yl)piperidin-3-yl)-3-methyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one hydrochloride as a white solid.
후처리
- customInto a 100-mL round-bottom flask, was placed
- customat room temperature
- temperatureThe resulting solution was heated
- temperatureto reflux overnight
- concentrationThe resulting mixture was concentrated under vacuum
- customThe resulting residue (150 mg) was purified by Prep-HPLC with the following conditions (Gilson Pre-HPLC)
출처 및 근거
- ORD 기록
- ord-ec50c70e4e5540698c9be724c786e5a0
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08822447B2
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