HRID1789023
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
PROCEDURE
实验过程
Trifluoroacetic anhydride (0.65 ml, 4.63 mmoles) was added with stirring to pyridine (0.75 ml, 9.26 mmoles) and diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(4-nitrophenyl)-3,5-pyridinedicarboxylate (2.31 g, 4.63 mmoles) in methylene chloride (60 ml). After stirring for 2.5 hours, the solution was washed with water, dilute hydrochloric acid (x3), water, saturated sodium bicarbonate solution, water and dried (Na2SO4). The solvent was removed in vacuo and the residue recrystallised from ethanol to give the title compound (1.77 g) as a yellow solid, mp 176°-7°.
WORKUP
后处理
- washthe solution was washed with water, dilute hydrochloric acid (x3), water, saturated sodium bicarbonate solution, water
- dry with materialdried (Na2SO4)
- customThe solvent was removed in vacuo
- customthe residue recrystallised from ethanol