HRID1491967

反应详情

EQUATION

反应方程式

HRID 1491967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(5-Octyl-2-pyridyl)phenol (0.5 g), 0.2 g of heptanoic acid and 0.04 g 4-(dimethylamino)pyridine were dissolved in 50 ml of dichloromethane and the solution was treated portion wise with 0.4 g of N,N'-dicyclohexylcarbodiimide within 10 minutes while stirring. The mixture was stirred at room temperature overnight and then filtered. The filtrate was diluted with dichloromethane, washed twice with 50 ml of saturated sodium carbonate solution each time and then with water, dried over magnesium sulphate, filtered and subsequently concentrated. The crude product obtained was purified by chromatography on silica gel with toluene. Recrystallization from ethanol gave 0.4 g of 4-(5-octyl-2-pyridyl)phenyl heptanoate with a m.p. (C--S) 57° C. and cl.p. (S--I) 77° C.

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature overnight
  2. filtrationfiltered
  3. additionThe filtrate was diluted with dichloromethane
  4. washwashed twice with 50 ml of saturated sodium carbonate solution each time
  5. dry with materialwith water, dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationsubsequently concentrated
  8. customThe crude product obtained
  9. customwas purified by chromatography on silica gel with toluene
  10. customRecrystallization from ethanol