HRID1608902

反应详情

EQUATION

反应方程式

HRID 1608902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.45 g (0.0016 moles) of 4-decyloxybenzoic acid and 0.58 g (0.0016 moles) of 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenol (prepared essentially as in Example 5) were dissolved in 25 ml of methylene chloride. N,N-dicyclohexylcarbodiimide (0.35 g, 0.0017 moles) was added to the reaction mixture, followed by 0.05 g of 4-(N,N-dimethylamino)pyridine. The resultant mixture was stirred at room temperature under nitrogen for 18 hours. The resulting urea precipitate was removed from the product solution by filtration, and the filtrate was concentrated on a rotary evaporator at reduced pressure. The crude product was purified by flash chromatography on silica gel (chloroform) to yield 0.12 g of 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenyl 4-decyloxybenzoate.

WORKUP

后处理

  1. customThe resulting urea precipitate was removed from the product solution by filtration
  2. concentrationthe filtrate was concentrated on a rotary evaporator at reduced pressure
  3. customThe crude product was purified by flash chromatography on silica gel (chloroform)