HRID2418260

反应详情

EQUATION

反应方程式

HRID 2418260 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 100 ml of benzene were dissolved 6 g of 2-nitratopropyl acetoacetate, 4.42 g of 3-nitrobenzaldehyde and 0.4 ml of piperidine. The solution was subjected to reflux, extraction, washing, dryness and evaporation of the solvent in the manner described in Example 9 to give a residue, to which 5.97 of 3-nitratopropyl 3-aminocrotonate was added. The mixture was treated in the manner described in Example 9 to give a residue, which was then subjected to column chromatography on silica gel (eluted with n-hexane-ethyl acetate=5:1) and recrystallized from ether to obtain 7.7 g of 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid 3-(2-nitratopropyl) ester-5-(3-nitratopropyl) ester.

WORKUP

后处理

  1. temperatureto reflux
  2. extractionextraction
  3. washwashing
  4. customdryness and evaporation of the solvent in the manner
  5. customto give a residue
  6. additionThe mixture was treated in the manner
  7. customto give a residue, which
  8. customrecrystallized from ether