HRID1608451

反应详情

EQUATION

反应方程式

HRID 1608451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.0 g (4.72×10-3 mol) of 5-hexylthiophene-2-carboxylic acid, 1.62 g (4.72×10-3 mol) 4-(5-undecyl-2-pyrimidinyl)-2-fluorophenol, N,N'-dicyclohexylcarbodiimide (DCC) and 0.03 g of pyrrolidinopyridine were dissolved in 30 ml of dichloromethane, followed by stirring overnight at room temperature. After the reaction, the insoluble matter was filtered off, followed by distilling-off of the solvent to obtain a crude product. The crude product was purified by silica gel column chromatography (eluent: toluene) and recrystallized from a mixture solvent (ethanol/ethyl acetate) to obtain 1.86 g of a pure product (Yield: 3.2%) ##STR84##

WORKUP

后处理

  1. customAfter the reaction
  2. filtrationthe insoluble matter was filtered off
  3. customto obtain a crude product
  4. customThe crude product was purified by silica gel column chromatography (eluent: toluene)
  5. customrecrystallized from a mixture solvent (ethanol/ethyl acetate)