反応式
[CH3:1][C@H:2]1[CH2:7][NH:6][C@H:5]([CH3:8])[CH2:4][NH:3]1.Cl[C:10]1[N:11]([CH2:32][CH:33]([CH3:35])[CH3:34])[C:12]2[C:17]([N:18]=1)=[C:16]([N:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1)[N:15]=[C:14]([C:25]1[CH:26]=[N:27][C:28]([NH2:31])=[N:29][CH:30]=1)[N:13]=2>CN1CCCC1=O>[CH3:1][C@H:2]1[CH2:7][NH:6][C@H:5]([CH3:8])[CH2:4][N:3]1[C:10]1[N:11]([CH2:32][CH:33]([CH3:35])[CH3:34])[C:12]2[C:17]([N:18]=1)=[C:16]([N:19]1[CH2:20][CH2:21][O:22][CH2:23][CH2:24]1)[N:15]=[C:14]([C:25]1[CH:26]=[N:27][C:28]([NH2:31])=[N:29][CH:30]=1)[N:13]=2参加物
4
反応条件
- 温度
- 150 °C
実験手順
trans-2,5-Dimethylpiperazine (150 mg, 1.3 mmol) and N-methylpyrrolidone (1 ml) were added to 5-(8-chloro-9-isobutyl-6-morpholin-4-yl-9H-purin-2-yl)pyrimidin-2-amine (100 mg, 0.26 mmol) and the resulting mixture was stirred at 150° C. for 48 hours. The reaction mixture was cooled and partitioned with methylene chloride and water, the organic layer was dried over magnesium sulfate, and the solvent was concentrated under reduced pressure. The residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid) to give the title compound (120 mg) as a pale yellow solid.
後処理
- temperatureThe reaction mixture was cooled
- custompartitioned with methylene chloride and water
- dry with materialthe organic layer was dried over magnesium sulfate
- concentrationthe solvent was concentrated under reduced pressure
- customThe residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid)
出典と根拠
- ORDレコード
- ord-85eb8076f55e404abe880280f47a8e3d
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08309546B2
関連ノート
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