HRID1769075
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
2M Sodium hydroxide (30 ml) was added to a solution of methyl 2,6-diethyl-1,4-dihydro-4-oxopyridine-3-carboxylate (obtained as described in European Patent Application No. 453210) in methanol (60 ml) and the solution was heated under reflux for 48 hours. Volatile material was removed by evaporation and the residue was dissolved in water (50 ml). The solution was washed with ethyl acetate and acidified to pH 4 with 1M citric acid solution. The resultant precipitate was collected by filtration to give 2,6-diethyl-1,4-dihydro-4-oxopyridine-3-carboxylic acid (E) (2.1 g), m.p. 238°-240° C. (decomposition); NMR (CDCl3): 1.3(t, 6H), 2.7(q, 2H), 3.3(q, 2H), 6.45(s, 1H), 12.1(br s, 1H).
WORKUP
后处理
- temperaturethe solution was heated
- temperatureunder reflux for 48 hours
- customVolatile material was removed by evaporation
- dissolutionthe residue was dissolved in water (50 ml)
- washThe solution was washed with ethyl acetate
- filtrationThe resultant precipitate was collected by filtration