反応式
Br[CH2:2][C:3]1[N:4]([CH3:19])[C:5]2[C:10]([N:11]=1)=[C:9]([N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1)[N:8]=[C:7]([Cl:18])[N:6]=2.[O:20]1[CH2:25][CH2:24][N:23]([CH:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH2:22][CH2:21]1.CCN(C(C)C)C(C)C>C(Cl)Cl>[Cl:18][C:7]1[N:6]=[C:5]2[C:10]([N:11]=[C:3]([CH2:2][N:29]3[CH2:30][CH2:31][CH:26]([N:23]4[CH2:24][CH2:25][O:20][CH2:21][CH2:22]4)[CH2:27][CH2:28]3)[N:4]2[CH3:19])=[C:9]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[N:8]=1参加物
5
実験手順
To a solution of 4-(8-(bromomethyl)-2-chloro-9-methyl-9H-purin-6-yl)morpholine (935 mg, 2.7 mmol) in DCM (30 mL) was added 4-morpholino-piperidine (505 mg, 2.97 mmol) and DIEA (0.70 mL). The resulting mixture was stirred at room temperature for 18 hours. The mixture was then poured onto water and the layers were separated. The aqueous layer was extracted with three times with DCM. The combined organic extracts were washed with water, dried over Na2SO4, filtered and concentrated. The crude product was then purified by flash chromatography (0-30% gradient MeOH in DCM) to give the title compound as a white solid (95%). LCMS: M+H+=436.2.
後処理
- additionThe mixture was then poured onto water
- customthe layers were separated
- extractionThe aqueous layer was extracted with three times with DCM
- washThe combined organic extracts were washed with water
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was then purified by flash chromatography (0-30% gradient MeOH in DCM)
出典と根拠
- ORDレコード
- ord-b862ae862dcf45b299df1ab5a96cd78c
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08158625B2
関連ノート
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