反应 #1509659

反应方程式

Sodium hydride

2-amino-6-chloro-9H-purine

2-iodopropane

→

title compound

2-Amino-6-chloro-9-isopropyl-9H-purine

溶剂

DMF

反应条件

后处理

1. 1
   温度the mixture was cooled in an ice bath
2. 2
   其他The cooling bath was removed
3. 3
   温度The mixture was cooled in ice
4. 4
   workup.ADDITIONwater was added
5. 5
   浓缩The mixture was concentrated
6. 6
   workup.ADDITIONthe residue was treated with hot ethyl acetate
7. 7
   过滤The cooled mixture was filtered
8. 8
   浓缩the filtrate was concentrated
9. 9
   其他The residue was purified by column chromatography on silica gel
10. 10
    洗涤eluting with 0 to 50% EtOAc in hexane

实验过程

Sodium hydride (1.5 g of 60% dispersion in mineral oil, 38 mmol) was added in portions over 10 min to a stirred suspension of 2-amino-6-chloro-9H-purine (5.34 g, 31.5 mmol) in anhydrous DMF (50 mL) at rt. After 45 min, the mixture was cooled in an ice bath, then 2-iodopropane was added. The cooling bath was removed and the stirred mixture was allowed to warm to rt over 16 h. The mixture was cooled in ice, then water was added. The mixture was concentrated, and the residue was treated with hot ethyl acetate. The cooled mixture was filtered, and the filtrate was concentrated. The residue was purified by column chromatography on silica gel, eluting with 0 to 50% EtOAc in hexane to afford the title compound as a solid. 1H NMR (400 MHz, CDCl3) δ 7.83 (s, 1H), 5.17 (s, 2H), 4.71-4.66 (m, 1H), 1.57 (d, 6H). MS m/z 212.1 (M+1).

来源