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