反応式
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([Cl:11])[N:3]=1.[H-].[Na+].Cl[CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20]>CN(C)C=O>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])=[C:4]([Cl:11])[N:3]=1参加物
5
実験手順
945 mg of 2,6-dichloropurine, 15 ml of DMF (dimethylformamide) and 288 mg of NaH are mixed and left at ambient temperature for 2 hours. 1.06 ml of 2-chloromethoxyethyltrimethylsilane are then added. The mixture is stirred for 18 hours at ambient temperature. The DMF is evaporated off. The product is taken up in methylene chloride. Washing is carried out with a saturated sodium bicarbonate solution and then once with H2O and, finally, with a saturated NaCl solution. Drying over Na2SO4 and evaporation to dryness are carried out. Purification is carried out by chromatography on silica with a CHCl3-AcOEt: 5-5 mixture for eluent. 876 mg of expected product are obtained, in the form of a yellow-colored oil.
後処理
- customThe DMF is evaporated off
- washWashing
- dry with materialDrying over Na2SO4 and evaporation to dryness
- customPurification
出典と根拠
- ORDレコード
- ord-9dae688878cc4cd98e06386b3760b190
- 出典データセット
- uspto-grants-2009_01
- 特許番号
- US07476670B2
関連ノート
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