HRID331389

反应详情

EQUATION

反应方程式

HRID 331389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Methoxy-3-phenyl-1H-inden-1-one (2.8 g, 11.85 mmol) obtained in Step 3 was placed into a flask and dissolved in CCl4 (20 mL). To the resulting solution, NBS (2.53 g, 14.22 mmol, 1.2 eq) and AIBN (280 mg, 10%/w) were added. The resulting mixture was allowed to reflux for 2 h. After cooling to room temperature, the reaction mixture was quenched with sat. Na2S2O3 (20 mL) extracted with CH2Cl2(20 mL×3). The organic layers were washed H2O and brine, dried over MgSO4 and concentrated in vacuo to give the desired product (2.45 g, 66%).

WORKUP

后处理

  1. temperatureto reflux for 2 h
  2. customthe reaction mixture was quenched with sat. Na2S2O3 (20 mL)
  3. extractionextracted with CH2Cl2(20 mL×3)
  4. washThe organic layers were washed H2O and brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo