HRID2102382

反应详情

EQUATION

反应方程式

HRID 2102382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customquenched by the addition of water (10 mL)
  2. additionEthyl acetate (50 mL) was added
  3. filtrationthe mixture was filtered
  4. washThe filtrate was washed with a saturated solution of sodium bicarbonate (40 mL)
  5. concentrationthe organics were concentrated
  6. custompurified by silica gel column chromatography (using 15% ethyl acetate/hexane as eluent)