反応式
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][C:19](=[O:26])[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:13](=[O:27])[N:12]([CH3:28])[C:11]=2[N:10]=[C:9]1Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:30]1[CH2:36][CH2:35][CH2:34][CH2:33][CH:32]([NH2:37])[CH2:31]1.C(N(CC)CC)C.O>CS(C)=O.ClCCl>[NH2:37][CH:32]1[CH2:33][CH2:34][CH2:35][CH2:36][N:30]([C:9]2[N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:16]3[C:15](=[O:17])[N:14]([CH2:18][C:19](=[O:26])[C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=4)[C:13](=[O:27])[N:12]([CH3:28])[C:11]=3[N:10]=2)[CH2:31]1参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
7-Benzyl-8-bromo-3-methyl-1-(2-oxo-2-phenylethyl)-3,7-dihydropurine-2,6-dione (77B) (227 mg, 0.5 mmol) and azepan-3-ylamine (342 mg, 3 mmol), and triethylamine (0.35 ml, 2.5 mmol) were dissolved in 20 ml of DMSO and the mixture was subjected to microwaves (method F, 100° C., 300 W) for five hours. To the reaction mixture was added 100 ml of water and 100 ml of dichloromethane, and the organic layer was separated and dried over sodium sulfate. The solvents were evaporated and the crude product was purified by preparative HPLC (method A1, Rt=8.77 min.). Evaporation of the solvent afforded the title compound as an yellow oil.
後処理
- customthe organic layer was separated
- dry with materialdried over sodium sulfate
- customThe solvents were evaporated
- customthe crude product was purified by preparative HPLC (method A1, Rt=8.77 min.)
- customEvaporation of the solvent
出典と根拠
- ORDレコード
- ord-ed957ddc3eed4bdb90a09ad4bb70cc2f
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07192952B2
関連ノート
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