反応式
[CH3:1][N:2]1[C:7](=[O:8])[CH:6]=[C:5]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][N:10]=2)[N:4]=[C:3]1[O:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:23]=[CH:24][C:25]3[N:30](COCC[Si](C)(C)C)[C:29](=[O:39])[O:28][CH2:27][C:26]=3[CH:40]=2)[CH2:18][CH2:17]1.Cl.O.C(=O)([O-])O.[Na+]>O1CCCC1>[CH3:1][N:2]1[C:7](=[O:8])[CH:6]=[C:5]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][N:10]=2)[N:4]=[C:3]1[O:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:23]=[CH:24][C:25]3[NH:30][C:29](=[O:39])[O:28][CH2:27][C:26]=3[CH:40]=2)[CH2:18][CH2:17]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 70 °C
実験手順
To a solution of 1-methyl-2-{[1-(2-oxo-1{[2-(trimethylsilyl)ethoxy]methyl}-1,4-dihydro-2H-3,1-benzoxazin-6-yl)piperidin-4-yl]oxy}-1H-[4,4′]bipyrimidinyl-6-one (78 mg, 0.14 mmol) in tetrahydrofuran (1.4 ml) was added 6N aqueous hydrochloric acid (1.4 ml, 8.4 mmol). The mixture was stirred at 70° C. for 3 hours. The mixture was poured into water. The aqueous solution was neutralized with sodium hydrogen carbonate. Extraction with dichloromethane was performed three times. The organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (eluent; chloroform/methanol=98/2) to afford 1-methyl-2-{[1-(2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)piperidin-4-yl]oxy}-1H-[4,4′]bipyrimidinyl-6-one as a pale yellow solid (22 mg, 0.051 mmol, 38%).
後処理
- extractionExtraction with dichloromethane
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography (eluent; chloroform/methanol=98/2)
出典と根拠
- ORDレコード
- ord-a70659b8e5af4006971f8fb1139a386c
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09006232B2
関連ノート
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