反应详情

A mixture of 9.0 g. (27 mmole) 9-[(2-benzoyloxyethoxy)-methyl]-6-chloropurine, 16.5 g. (81 mmole) N-cyclopentyl-(2,5-dimethylbenzyl)-amine and 130 ml. butanol is heated under reflux for 16 hours. The reaction mixture is evaporated, the residue is taken up in dichloromethane, washed with dilute acetic acid and subsequently with water, dried over anhydrous sodium sulphate, evaporated, mixed with a solution of 3.3 g. sodium in 200 ml. methanol, heated under reflux for 3 hours, evaporated and the residue taken up in water, extracted with dichloromethane, dried over anhydrous sodium sulphate and evaporated. After chromatography on silica gel with an elution mixture of 95% dichloromethane and 5% methanol, there are obtained 8.0 g. of the title compound (75% of theory) in the form of an oily base, the hydrochloride of which, prepared in ethyl acetate, melts at 132°-135° C.

1. additionA mixture of 9.0 g
2. temperatureunder reflux for 16 hours
3. customThe reaction mixture is evaporated
4. washwashed with dilute acetic acid and subsequently with water
5. dry with materialdried over anhydrous sodium sulphate
6. customevaporated
7. additionmixed with a solution of 3.3 g
8. temperaturemethanol, heated
9. temperatureunder reflux for 3 hours
10. customevaporated
11. extractionextracted with dichloromethane
12. dry with materialdried over anhydrous sodium sulphate
13. customevaporated
14. additionAfter chromatography on silica gel with an elution mixture of 95% dichloromethane and 5% methanol, there
15. customare obtained 8.0 g