Acetic Anhydride → HCID 20773484、化合物
反応式
[CH2:1]([O:8][CH2:9][C:10]1[NH:18][C:17]2[C:16](=[O:19])[N:15]([CH2:20][CH2:21][CH2:22][CH2:23][C@H:24]([OH:26])[CH3:25])[C:14](=[O:27])[N:13]([CH3:28])[C:12]=2[N:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:36](OC(=O)C)(=[O:38])[CH3:37]>CN(C)C1C=CN=CC=1.C(Cl)(Cl)Cl>[C:36]([O:26][C@H:24]([CH3:25])[CH2:23][CH2:22][CH2:21][CH2:20][N:15]1[C:16](=[O:19])[C:17]2[NH:18][C:10]([CH2:9][O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[N:11][C:12]=2[N:13]([CH3:28])[C:14]1=[O:27])(=[O:38])[CH3:37]参加物
実験手順
To a stirred solution of (R)-8-benzyloxymethyl-1-(5-hydroxyhexyl)-3-methylxanthine (19.9 g, 51.5 mmol), triethylamine (10.4 g, 103 mmol) and 4-dimethylaminopyridine (1.33 g, 11 mmol) in chloroform (130 ml) was added acetic anhydride (6.57 g, 64.4 mmol). After stirring for 3 hours at room temperature, the reaction mixture was quenched by addition of methanol (5 ml). The mixture was washed with aqueous potassium hydrogen sulfate solution (0.1 N) to pH 6-7, with water (2×50 ml) and with saturated aqueous sodium chloride solution (50 ml). After drying over magnesium sulfate, the organic solution was evaporated under reduced pressure to provide (R)-1-(5-acetoxyhexyl)-8-benzoxymethyl-3-methylxanthine (19.6 g, 88% yield) as white colored solid.
後処理
- customthe reaction mixture was quenched by addition of methanol (5 ml)
- washThe mixture was washed with aqueous potassium hydrogen sulfate solution (0.1 N) to pH 6-7, with water (2×50 ml) and with saturated aqueous sodium chloride solution (50 ml)
- dry with materialAfter drying over magnesium sulfate
- customthe organic solution was evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-ae29cbcdc467440fa6191f0cea0f8d67
- 出典データセット
- uspto-grants-2005_04
- 特許番号
- US06878715B1
反応ノート
読み込み中…