HRID1010930

反应详情

EQUATION

反应方程式

HRID 1010930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturecooled to 50° C
  2. temperaturethe reaction heated to 50° C. overnight
  3. waitat 90° C. for 2 hours
  4. washwashed with water (10 ml)
  5. customThe organic layer was separated
  6. concentrationconcentrated in vacuo
  7. customto afford