HRID1899075

反应详情

EQUATION

反应方程式

HRID 1899075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Titanium (IV) chloride (2.7 ml) was added dropwise to a stirred solution of 2-(4-fluorophenyl)-3-[4-(methylsulfonyl)phenyl]thiophene (5 g) and acetyl chloride (2.2 ml) in benzene (50 ml) at 5° to 10° C. The mixture was stirred at ambient temperature for 4 hours, poured into ice-water, and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium bicarbonate, dried and concentrated. The residue was recrystallized from a mixture of ethanol and ethyl acetate to give pale brown crystals of 5-acetyl-2-(4-fluorophenyl)-3-[4-(methylsulfonyl)phenyl]thiophene (3.7 g).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with an aqueous solution of sodium bicarbonate
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from a mixture of ethanol and ethyl acetate