HRID1011107

反应详情

EQUATION

反应方程式

HRID 1011107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 2-[(2-cyclopropylethyl)oxy]-8-(methyloxy)-1H-purin-6-amine trifluoroacetate (0.16 g, 0.450 mmol) and anhydrous potassium carbonate (0.243 g, 1.762 mmol) in DMF (2.5 ml) was heated at 50° C. for 1 hour. The mixture was cooled to room temperature and 3-(2-bromoethyl)tetrahydrofuran (0.095 g, 0.528 mmol) was added and the mixture heated at 50° C. for 18 hours. The mixture was quenched with water (2 ml) and extracted with DCM (2×5 ml). The DCM was separated through a hydrophobic frit and evaporated by blowing down under a stream of nitrogen. The sample was dissolved in 1:1 MeOH:DMSO (3×0.5 ml) and purified by mass directed autopreparation. Product containing fractions were evaporated under a stream of nitrogen in a blowdown apparatus to give the title compound as a white solid (98 mg).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. temperaturethe mixture heated at 50° C. for 18 hours
  3. customThe mixture was quenched with water (2 ml)
  4. extractionextracted with DCM (2×5 ml)
  5. customThe DCM was separated through a hydrophobic frit
  6. customevaporated
  7. dissolutionThe sample was dissolved in 1:1 MeOH
  8. customDMSO (3×0.5 ml) and purified by mass
  9. additionProduct containing fractions
  10. customwere evaporated under a stream of nitrogen in a blowdown apparatus