HRID747868

反应详情

EQUATION

反应方程式

HRID 747868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 7-methoxy-3-(6-methoxy-pyridin-3-yl)-4-methyl-chromen-2-one in CH2Cl2 (5 mL) at room temperature was added BBr3 (1.0 N, 24.2 mmoL, 24 mL) dropwise. After addition, the reaction was slightly heated to reflux 4 hours. The reaction was quenched with ice sat. NaHCO3, extracted with 3×CH2Cl2, washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the crude material. The crude material was re-crystallized in 2:1 hexanes:ethyl acetate to afford the title product as a pale reddish solid.

WORKUP

后处理

  1. additionAfter addition
  2. temperaturethe reaction was slightly heated
  3. temperatureto reflux 4 hours
  4. customThe reaction was quenched with ice sat. NaHCO3
  5. extractionextracted with 3×CH2Cl2
  6. washwashed with brine
  7. dry with materialdried over anhydrous Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customto give the crude material
  11. customThe crude material was re-crystallized in 2:1 hexanes