HRID4324
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Ethyl veratroylacetate (4.5 g) was added dropwise under stirring at 60°-70° C. to a suspension of 2-aminopyridine (0.84 g) in polyphosphoric acid (13.7 g). The reaction mixture was stirred at 100° C. for 3 hrs and poured into ice-water (50 ml). The aqueous solution was extracted with chloroform, washed with water, dried and evaporated to give dark oily residue which was chromatographed on silica gel using n-hexaneethyl acetate. The fractions were evaporated and the resulting residue was triturated with ethanol-isopropyl ether to give 2-(3,4-dimethoxyphenyl)-4-oxo-4H-pyrido[1,2-a]pyrimidine (3.8 g).
WORKUP
后处理
- extractionThe aqueous solution was extracted with chloroform
- washwashed with water
- customdried
- customevaporated
- customto give dark oily residue which
- customwas chromatographed on silica gel using n-hexaneethyl acetate
- customThe fractions were evaporated
- customthe resulting residue was triturated with ethanol-isopropyl ether