反応式
[Cl:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[NH:4][CH:5]=[N:6]2.[H-].[Na+].[C:13]([O:16][CH2:17][CH2:18][O:19][CH2:20]Br)(=[O:15])[CH3:14].O>CN(C=O)C>[C:13]([O:16][CH2:17][CH2:18][O:19][CH2:20][N:6]1[CH:5]=[N:4][C:3]2[C:7]1=[N:8][CH:9]=[N:10][C:2]=2[Cl:1])(=[O:15])[CH3:14]参加物
6
実験手順
To a solution of 6-chloropurine (6 g, 38.8 mmoles) in DMF was added sodium hydride 60% (0.93 g) over 1.5 hour period. (2-acetoxyethoxy)methyl bromide was then added at room temperature; the reaction mixture was allowed to stir for 2 hours under Nz atmosphere. H2O was added and the product was extracted with ethyl acetate. The organic phase was dried over MgSO4, filtered, and evaporated in vacuo to give a light yellow solid 7.1 g, 68% yield of 9-[(2-acetoxy-ethoxy)methyl]-6-chloro-purine. The crude was used without further purification.
後処理
- extractionthe product was extracted with ethyl acetate
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-f44e10d4426d48e2be129f56c37ce4e1
- 出典データセット
- uspto-grants-1992_06
- 特許番号
- US05117830
関連ノート
読み込み中…