HRID371414
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
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
- temperatureuder reflux for 6 hours
- temperatureAfter cooling
- distillationthe solvent was distilled off in vacuo
- customwas chromatographed on a silica gel column
- additionwith the addition of methanol
- additionThe fractions containing the product
- concentrationwere concentrated
- customthe nitrodihydropyridine crystallized in yellow crystals of melting point 161° C.