反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe organic phase is then separated
- extractionthe aqueous phase is extracted with 2×20 ml ethyl acetate
- dry with materialAfter the combined organic phases have been dried over sodium sulfate
- customthe solvents are evaporated
- additionTreatment of the residue with a solvent mixture of THF and hexane in a ratio by volume of 1:20