反応式
[C:1]1([CH:7]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([C:19]([O:21]CC)=[O:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][N:14]3[CH:24]2[CH2:29][CH2:28][CH2:27][CH2:26][O:25]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[OH-].[Na+].Cl>ClCCl>[C:30]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([C:19]([OH:21])=[O:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][N:14]3[CH:24]2[CH2:29][CH2:28][CH2:27][CH2:26][O:25]2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a suspension of ethyl 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carboxylate (0.55 g, 1.16 mmol) (Preparation 27) in industrial methylated spirits (2.2 ml) was added deionised water (0.08 ml) followed by 10 M aqueous sodium hydroxide solution (0.23 ml, 2.3 mmol). The resultant mixture was stirred at 65° C. for 30 minutes and then at ambient temperature for 18 hours during which time a thick paste was formed. To this mixture was added dichloromethane (10 ml) and the pH was adjusted to 2 by the addition of dilute aqueous hydrochloric acid solution. The phases were separated and the aqueous layer was extracted with dichloromethane (10 ml). The combined organic phases were then dried (MgSO4) and the solvent was removed under reduced pressure to give the title compound as a tan coloured foam (0.43 g) that was identical by 1H-NMR, high performance liquid chromatography, mass spectrometry and thin-layer chromatography to the compound prepared in Preparation 21.
後処理
- customat ambient temperature for 18 hours during which time a thick paste was formed
- customThe phases were separated
- extractionthe aqueous layer was extracted with dichloromethane (10 ml)
- dry with materialThe combined organic phases were then dried (MgSO4)
- customthe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-e486f1fec2da4c259963ca371edee487
- 出典データセット
- uspto-grants-2005_05
- 特許番号
- US06900309B1
関連ノート
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