HRID422001
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
- 170 °C
PROCEDURE
实验过程
To a flask were added DBU (20 mL) and (R,E)-ethyl 3-(2-amino-4-methyl-6-(tetrahydrofuran-3-ylamino)pyrimidin-5-yl)acrylate (3.9 g, 13.4 mmol). The reaction mixture was stirred at 170° C. for 24 h under nitrogen. The mixture was allowed to cool to room temperature and was diluted with water. The aqueous layer was extracted with ethyl acetate (100 mL×3). The combined organic layers were washed with brine, separated and dried with MgSO4. The mixture was purified by chromatography to give (R)-2-amino-4-methyl-8-(tetrahydrofuran-3-yl)pyrido[2,3-d]pyrimidin-7(8H)-one (1.59 g, 48% yield); MS (EI) for C12H14N4O2: 247.1 (MH+).
WORKUP
后处理
- temperatureto cool to room temperature
- extractionThe aqueous layer was extracted with ethyl acetate (100 mL×3)
- washThe combined organic layers were washed with brine
- customseparated
- dry with materialdried with MgSO4
- customThe mixture was purified by chromatography