反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
10 g. triacetyl-6-chloro-9-(β-D-ribofuranosyl)-purine and 10 g. allyl-cyclohexylamine were heated under reflux for 1 hour in 100 ml. butanol. The butanol was then distilled off in a vacuum, the residue was dissolved in chloroform and the chloroform solution was then shaken out successively with dilute hydrochloric acid, dilute aqueous sodium bicarbonate solution and water. The chloroform solution was then dried over anhydrous sodium sulfate and evaporated to a syrup. This was dissolved in methanol and the solution, after the addition of 5 ml. 1N sodium methylate solution was heated for 10 minutes on a steambath. After cooling, the solution was distilled off to dryness, the residue was dissolved in chloroform and the chloroform solution was washed with water. The organic phase was dried and evaporated and the residue obtained recrystallized from ethanol. 6.1 g. (59% of theory) N(6)-allyl-N(6)-cyclohexyl-adenosine were obtained; m.p. 123° - 125° C.
WORKUP
后处理
- temperatureunder reflux for 1 hour in 100 ml
- distillationThe butanol was then distilled off in a vacuum
- dissolutionthe residue was dissolved in chloroform
- dry with materialThe chloroform solution was then dried over anhydrous sodium sulfate
- customevaporated to a syrup
- dissolutionThis was dissolved in methanol
- additionthe solution, after the addition of 5 ml
- temperature1N sodium methylate solution was heated for 10 minutes on a steambath
- temperatureAfter cooling
- distillationthe solution was distilled off to dryness
- dissolutionthe residue was dissolved in chloroform
- washthe chloroform solution was washed with water
- customThe organic phase was dried
- customevaporated
- customthe residue obtained
- customrecrystallized from ethanol