Potassium Carbonate → HCID 9801004、化合物

反応式

[NH:1]1[CH2:7][CH:6]([CH2:8][OH:9])[CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:10]([N:17]1[C:25]2[C:24](=[O:26])[N:23]([CH3:27])[C:22](=[O:28])[N:21]([CH3:29])[C:20]=2[N:19]=[C:18]1Cl)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:10]([N:17]1[C:25]2[C:24](=[O:26])[N:23]([CH3:27])[C:22](=[O:28])[N:21]([CH3:29])[C:20]=2[N:19]=[C:18]1[N:1]1[CH2:7][CH:6]([CH2:8][OH:9])[CH2:5][NH:4][CH2:3][CH2:2]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

実験手順

([1,4]Diazepan-6-yl)methanol (1C) including potassium carbonate salts (ca 1 mmol) was suspended in dry DMF (200 ml) and 7-benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-purine-2,6-dione (199.9 mg, 0.656 mmol) and potassium carbonate (453 mg, 3.28 mmol) were added. The reaction mixture was stirred at room temperature for 24 hours, heated to 60° C. for 3 hours, heated to 95° C. for 5 hours and heated to 120° C. for 2 hours. The suspension was allowed to cool to room temperature and white salts were filtered off. The filtrate was evaporated and purified by chromatography on silica, using 5% methanol in dichloromethane as the eluent. Fractions containing the product were evaporated and purified by preparative HPLC (method A2; Rt=2.52 min.) to afford 8 mg of the title compound as an yellow oil in 1% yield.