HRID1789023

反应详情

EQUATION

反应方程式

HRID 1789023 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washthe solution was washed with water, dilute hydrochloric acid (x3), water, saturated sodium bicarbonate solution, water
  2. dry with materialdried (Na2SO4)
  3. customThe solvent was removed in vacuo
  4. customthe residue recrystallised from ethanol