HRID574657
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
- 80 °C
PROCEDURE
实验过程
To a mixture of product of step C, compound 1-1-c, (1.2 g, 2.4 mmol), ethyl methyl-phosphite (522 mg, 4.8 mmol) and Et3N (610 mg, 6 mmol) in DMF (20 mL) was added PdCl2(dppf) (176 mg). The mixture was allowed to stir overnight at 80° C. The mixture was cooled to room temperature and diluted with water. The resulting mixture was then filtered and the filtrate was extracted with dichloromethane/methanol (5/1). The organic layer was dried over sodium sulfate and concentrated under vacuum. And the residue was purified over silica gel (dichloromethane:methanol=3/1) to provide the product, 1-1-d, (500 mg, 44%).
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- filtrationThe resulting mixture was then filtered
- extractionthe filtrate was extracted with dichloromethane/methanol (5/1)
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated under vacuum
- customAnd the residue was purified over silica gel (dichloromethane:methanol=3/1)
- customto provide the product, 1-1-d, (500 mg, 44%)