Water → 2-(5-phenyl-[1,4]oxazepane-4-yl)-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one
반응식
Cl.[C:2]1([CH:8]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10][NH:9]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:16]1[N:21]([CH3:22])[C:20](=[O:23])[CH:19]=[C:18]([C:24]2[CH:29]=[CH:28][N:27]=[CH:26][N:25]=2)[N:17]=1.C(N(CC)CC)C.O>O1CCCC1>[C:2]1([CH:8]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10][N:9]2[C:16]2[N:21]([CH3:22])[C:20](=[O:23])[CH:19]=[C:18]([C:24]3[CH:29]=[CH:28][N:27]=[CH:26][N:25]=3)[N:17]=2)[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1참가 물질
반응 조건
- 온도
- 150 °C
실험 절차
To a suspension of 5-phenyl-[1,4]oxazepane hydrochloride (0.07 g, 0.33 mmol) and 2-chloro-3-methyl-6-(pyrimidin-4-yl)-3H-pyrimidin-4-one (0.07 g, 0.30 mmol) in tetrahydrofuran (2 mL) in a sealed tube was added triethylamine (0.14 mL) at room temperature. The mixture was heated to 150° C. under microwave irradiation and stirred for 15 min. After cooling to room temperature, the reaction mixture was poured into water and extracted with chloroform. The extracts were dried over anhydrous sodium sulfate and concentrated. The residue was purified by flash column chromatography on silica gel (chloroform/methano=10/1 as an eluant) to yield 2-(5-phenyl-[1,4]oxazepane-4-yl)-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one (A071) (0.07 g, 0.20 mmol, 66%) as a white solid.
후처리
- temperatureAfter cooling to room temperature
- extractionextracted with chloroform
- dry with materialThe extracts were dried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe residue was purified by flash column chromatography on silica gel (chloroform/methano=10/1 as an eluant)
출처 및 근거
- ORD 기록
- ord-fd64d189fda1453eb9963e889c4044ae
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09108957B2
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