HRID485075

反应详情

EQUATION

反应方程式

HRID 485075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5.1 grams of diisopropyl 1-(3-nitrobenzylidene)-acetonylphosphonate and 2.69 grams of 2-n-propoxyethyl 3-aminocrotonate was added to 20 ml of isopropanol and the mixture was heated to reflux for eight hours with stirring. The reaction mixture was evaporated in vacuo, to the residue was added ether to crystallize, the crystals were collected by filtration, and recrystallized from a mixture of ethyl acetate and ether to afford 5.38 grams of 2-n-propoxyethyl 2,6-dimethyl-4-(3-nitrophenyl)-5-diisopropoxyphosphinyl-1,4-dihydropyridine-3-carboxylate, pale yellow crystals, melting point 125°-6° C. Yield 72%.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for eight hours
  3. customThe reaction mixture was evaporated in vacuo, to the residue
  4. additionwas added ether
  5. customto crystallize
  6. filtrationthe crystals were collected by filtration
  7. customrecrystallized from a mixture of ethyl acetate and ether