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
- 0 °C
PROCEDURE
实验过程
To a solution of 3-(difluoromethyl)-5-(2-(3,5-dimethyl-1-tosyl-1H-indazol-4-yl)-4-methoxy-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-1-methyl-1H-pyrazole-4-carbaldehyde (0.8 g, 1.287 mmol) in ethanol (10.7 mL) was added concentrated HCl (2.1 mL). The microwave vessel was sealed and the mixture was irradiated at 125° C. for 1 h 20 min. The reaction mixture was then cooled to 0° C. and poured into ice water. Solid sodium bicarbonate was slowly added to neutralize the reaction mixture to pH=7, then the crude product was extracted with DCM (3×) and the combined organic layers were dried over sodium sulfate to provide 6-(3-(difluoromethyl)-1-methyl-1H-pyrazol-5-yl)-2-(3,5-dimethyl-1H-indazol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-ol, MS (ESI+) m/z 426.4 (M+H)+.
WORKUP
后处理
- customThe microwave vessel was sealed
- customthe mixture was irradiated at 125° C. for 1 h 20 min
- extractionthe crude product was extracted with DCM (3×)
- dry with materialthe combined organic layers were dried over sodium sulfate