HRID1010932

反应详情

EQUATION

反应方程式

HRID 1010932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

2-Butoxy-8-methoxy-9H-purin-6-amine trifluoroacetate salt (0.20 g) was dissolved in anhydrous N,N-dimethylformamide (5 mL) was treated with anhydrous potassium carbonate (0.315 g), heated to 60° C. for 1 hour and then cooled to room temperature. To the above was added 3-(bromomethyl)tetrahydrofuran (0.103 g) and the reaction mixture heated at 50° C., overnight. The reaction mixture was quenched with water (25 mL) and extracted into ethyl acetate (3 times, 100 mL combined total volume). The combined organic phase was separated and passed through a hydrophobic frit to dry. The organic phase was stripped to give a gum which was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (20-60%) to afford the title compound as a white solid (97 mg).

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. temperaturethe reaction mixture heated at 50° C., overnight
  3. customThe reaction mixture was quenched with water (25 mL)
  4. extractionextracted into ethyl acetate (3 times, 100 mL combined total volume)
  5. customThe combined organic phase was separated
  6. customto dry
  7. customto give a gum which
  8. customwas purified by C18 reverse phase chromatography