HRID485075
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureto reflux for eight hours
- customThe reaction mixture was evaporated in vacuo, to the residue
- additionwas added ether
- customto crystallize
- filtrationthe crystals were collected by filtration
- customrecrystallized from a mixture of ethyl acetate and ether