反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:8]1[N:9]([CH2:30][CH:31]([CH3:33])[CH3:32])[C:10]2[C:15]([N:16]=1)=[C:14]([N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1)[N:13]=[C:12]([C:23]1[CH:24]=[N:25][C:26]([NH2:29])=[N:27][CH:28]=1)[N:11]=2>CN1CCCC1=O>[CH2:30]([N:9]1[C:8]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)=[N:16][C:15]2[C:10]1=[N:11][C:12]([C:23]1[CH:28]=[N:27][C:26]([NH2:29])=[N:25][CH:24]=1)=[N:13][C:14]=2[N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1)[CH:31]([CH3:33])[CH3:32]参加物
4
反応条件
- 温度
- 130 °C
実験手順
Piperazine (2.0 g, 23 mmol) and N-methylpyrrolidone (10 ml) were added to 5-(8-chloro-9-isobutyl-6-morpholin-4-yl-9H-purin-2-yl)pyrimidin-2-amine (1.0 g, 2.6 mmol) and the resulting mixture was stirred at 130° C. for 4 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. This compound (10 ml in liquid) was stored with N-methylpyrrolidone remaining and used for next step.
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
出典と根拠
- ORDレコード
- ord-0beadc145db84d479a8e0c6abae201dd
- 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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