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
- 90 °C
PROCEDURE
实验过程
A mixture of 3-(2-chloropyrimidin-4-yl)-7-(1-methyl-1-triethylsilanyloxyethyl)imidazo[1,2-α]pyrimidine (from Example 34) (200 mg, 0.49 mmol), 3-furanboronic acid (111 mg, 0.98 mmol), K3PO4 (457 mg, 1.96 mmol) and tetrakis(triphenylphosphine)palladium(0) (50 mg, 9 mol %) in DMA (6 ml) was heated at 90° C. for 45 min under N2. The reaction was concentrated under reduced pressure while azeotroping with xylene (3×30 ml). EtOAc (50 ml) and H2O (50 ml) were added and the organics separated and concentrated under reduced pressure while loading onto MgSO4. Purification by column chromatography on silica using 3% MeOH/CH2Cl2 as the eluent gave 3-[2-(furan-3-yl)pyrimidin-4-yl]-7-(1-methyl-1-triethylsilanyloxyethyl)imidazo[1,2-α]pyrimidine (203 mg, 94%): m/z (ES+) 435 (M+H+).
WORKUP
后处理
- concentrationThe reaction was concentrated under reduced pressure
- customwhile azeotroping with xylene (3×30 ml)
- additionEtOAc (50 ml) and H2O (50 ml) were added
- customthe organics separated
- concentrationconcentrated under reduced pressure
- customPurification by column chromatography on silica using 3% MeOH/CH2Cl2 as the eluent