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
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To a solution of N2-butyl-8-methoxy-9H-purine-2,6-diamine trifluoroacetic acid salt (400 mg) in dry N,N-dimethylformamide (6 ml) at room temperature and under nitrogen was added potassium carbonate (630 mg) in one go. The reaction was stirred at 60° C. for 1.5 hours and then cooled to 50° C. 2-(Bromomethyl)tetrahydro-2H-pyran (175 μl) was added in one go and the reaction heated to 50° C. overnight and then at 90° C. for 2 hours. The reaction was diluted with ethyl acetate (20 ml) and washed with water (10 ml). The organic layer was separated and concentrated in vacuo. The product was semi-purified by MDAP to afford a mixture of the title compound and an isomer. This mixture was taken on without further purification.
WORKUP
后处理
- temperaturecooled to 50° C
- temperaturethe reaction heated to 50° C. overnight
- waitat 90° C. for 2 hours
- washwashed with water (10 ml)
- customThe organic layer was separated
- concentrationconcentrated in vacuo
- customto afford