HRID1650633

反应详情

EQUATION

反应方程式

HRID 1650633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In pyridine was dissolved 2 g of p-octyloxyphenol, and a solution of p-acetoxybenzoic acid chloride in chloroform was added dropwise to the thus-obtained solution and the mixture was stirred at room temperature for 3 hours. Water was added to the thus-obtained solution and the mixture was extracted with chloroform, and the extract was washed with a 0.5N aqueous solution of hydrochloric acid, a saturated aqueous solution of sodium chloride, a saturated aqueous solution of NaHCO3 and a saturated aqueous solution of sodium chloride in succession, followed by concentration. The concentrate was recrystallized from n-hexane to obtain 2.35 g of 4-octyloxyphenyl 4-acetoxybenzoate. The product was dissolved in a liquid mixture comprising tetrahydrofuran and methanol at a volume ratio of 10/1, 6.2 ml of a 1N aqueous solution of lithium hydroxide was added to the solution, the mixture was stirred at room temperature for 1 hour, and the mixture was diluted with ethyl acetate and washed with a saturated aqueous solution of sodium chloride. Then, the liquid was dehydrated on anhydrous magnesium sulfate and concentrated, and the concentrate was recrystallized from ethyl acetate to obtain 1.1 g of 4-octyloxyphenyl 4-hydroxybenzoate.

WORKUP

后处理

  1. extractionthe mixture was extracted with chloroform
  2. washthe extract was washed with a 0.5N aqueous solution of hydrochloric acid
  3. concentrationa saturated aqueous solution of sodium chloride, a saturated aqueous solution of NaHCO3 and a saturated aqueous solution of sodium chloride in succession, followed by concentration
  4. customThe concentrate was recrystallized from n-hexane