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
PROCEDURE
实验过程
3-Butenylmagnesium bromide (0.0040 mol) was added to a solution of 4-chloro-5-(4-fluorophenyl)thieno[2,3-d]pyrimidine (0.529 g, 0.00200 mol), copper (I) iodide (0.038 g, 0.00020 mol) and ferrous bromide (0.043 g, 0.00020 mol) in tetrahydrofuran (10 mL) and the resulting mixture was maintained at room temperature for 5 h, then quenched by the addition of water (10 mL). Ethyl acetate (50 mL) was added and the mixture was filtered. The filtrate was washed with a saturated solution of sodium bicarbonate (40 mL) and the organics were concentrated and purified by silica gel column chromatography (using 15% ethyl acetate/hexane as eluent) to afford 4-But-3-en-1-yl-5-(4-fluorophenyl)thieno[2,3-d]pyrimidine as a white solid in 67% yield.
WORKUP
后处理
- customquenched by the addition of water (10 mL)
- additionEthyl acetate (50 mL) was added
- filtrationthe mixture was filtered
- washThe filtrate was washed with a saturated solution of sodium bicarbonate (40 mL)
- concentrationthe organics were concentrated
- custompurified by silica gel column chromatography (using 15% ethyl acetate/hexane as eluent)