HRID414579

反应详情

EQUATION

反应方程式

HRID 414579 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1.52 gram (0.008 mole) of 2-formyl-5-phenylthiophene and 2.0 grams (0.00820 mole) of diethyl 4-methylbenzylphosphonate in 40 mL of N,N-dimethylformamide was added 0.53 gram (0.0098 mole) of sodium methoxide. The reaction mixture was stirred at room temperature for approximately 18 hours and then was quenched with 50 mL of an aqueous solution saturated with ammonium chloride. A precipitate formed and was collected by filtration. The filter cake was washed with water. The washed solid was purified by column chromatography on silica gel, eluting with chloroform:n-hexane (10:90) yielded 1.1 gram of 2-(4-methylphenyl)-1-(5-phenylthien-2-yl)ethene as a solid, m.p. 159°-160° C.

WORKUP

后处理

  1. customwas quenched with 50 mL of an aqueous solution saturated with ammonium chloride
  2. customA precipitate formed
  3. filtrationwas collected by filtration
  4. washThe filter cake was washed with water
  5. customThe washed solid was purified by column chromatography on silica gel
  6. washeluting with chloroform:n-hexane (10:90)