HRID371413

反应详情

EQUATION

反应方程式

HRID 371413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.1 g (0.1 mol) of 3-nitrobenzaldehyde, together with 16.9 g (0.1 mol) of cyclopentyl β-aminocrotonate and 10.3 g (0.1 mol) of nitroacetone in 150 ml of ethanol, were heated under reflux for 6 hours. After the reaction mixture had cooled, the solvent was distilled off in vacuo, and the oily residue was taken up in a small amount of chloroform and was chromatographed on a silica gel column, using chloroform with the addition of methanol. The fractions containing the reaction product were concentrated, the residue was taken up in a small amount of isopropanol, and the nitrodihydropyridine crystallized in yellow crystals of melting point 174° C.

WORKUP

后处理

  1. temperatureunder reflux for 6 hours
  2. temperatureAfter the reaction mixture had cooled
  3. distillationthe solvent was distilled off in vacuo
  4. customwas chromatographed on a silica gel column
  5. additionwith the addition of methanol
  6. additionThe fractions containing the reaction product
  7. concentrationwere concentrated
  8. customthe nitrodihydropyridine crystallized in yellow crystals of melting point 174° C.