HRID371414

反应详情

EQUATION

反应方程式

HRID 371414 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 18.8 g (0.1 mol) of β-n-propoxyethyl acetoacetate and 10.2 g (0.1 mol) of 2-amino-1-nitro-prop-1-ene in 150 ml of ethanol, were heated uder reflux for 6 hours. After cooling, 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 product were concentrated, the residue was taken up in a small amount of isopropanol, and the nitrodihydropyridine crystallized in yellow crystals of melting point 161° C.

WORKUP

后处理

  1. temperatureuder reflux for 6 hours
  2. temperatureAfter cooling
  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 product
  7. concentrationwere concentrated
  8. customthe nitrodihydropyridine crystallized in yellow crystals of melting point 161° C.