HRID1959125

反应详情

EQUATION

反应方程式

HRID 1959125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pyridinium bromide perbromide (1.00 g) was added to a solution of 7-chloro-4-(4-fluorophenyl)-2,2-dimethyl-2H-chromen (a compound obtained in Reference Example 5(3); 1.00 g) in dichloromethane (15 mL) under ice-cooling and the mixture was stirred at room temperature for 1.5 hours. The reaction mixture was poured into a 15% aqueous solution of sodium thiosulfate and extracted with ethyl acetate. The organic layer was washed successively with a saturated solution of sodium bicarbonate and brine, dried over sodium sulfate and concentrated in vacuo. The resultant residue was purified by column chromatography on silica gel (Solvent: n-hexane/chloroform=100/0 to 95/5) to give the titled compound (1.26 g) as a colorless powder.

WORKUP

后处理

  1. customobtained in Reference Example 5(3)
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed successively with a saturated solution of sodium bicarbonate and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant residue was purified by column chromatography on silica gel (Solvent: n-hexane/chloroform=100/0 to 95/5)