HRID1609709

反应详情

EQUATION

反应方程式

HRID 1609709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 12.7 g (12.2 mmol) 1,3-O-dicarbotrichloroethoxy-4-O-dicarbotrichloroethoxycaffeoyl quinide in 870 ml THF is treated for 3 days with 9 ml concentrated HCl. After cooling to 0° C., the reaction mixture is adjusted to pH 2 by addition of solid sodium bicarbonate and is then saturated with NaCl. The organic phase is then separated and the aqueous phase is extracted with 2×20 ml ethyl acetate. After the combined organic phases have been dried over sodium sulfate, the solvents are evaporated. Treatment of the residue with a solvent mixture of THF and hexane in a ratio by volume of 1:20 gives 12.7 g 1,3-O-dicarbotrichloroethoxy- 4-O-dicarbotrichloroethoxycaffeoyl quinic acid in the form of an amorphous white powder (yield 99%) .

WORKUP

后处理

  1. customThe organic phase is then separated
  2. extractionthe aqueous phase is extracted with 2×20 ml ethyl acetate
  3. dry with materialAfter the combined organic phases have been dried over sodium sulfate
  4. customthe solvents are evaporated
  5. additionTreatment of the residue with a solvent mixture of THF and hexane in a ratio by volume of 1:20