HRID1579447
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 16.5 g of ethyl 2-cyano-2-(5-oxo-5H-[1]benzopyrano-[2,3-b]pyridin-7-yl)propionate, 80 ml of acetic acid and 35 ml of concentrated hydrochloric acid is heated under reflux for 24 hours. After concentration, water is added to the residue, and further a 10% sodium hydroxide solution is added to dissolve the residue. An insoluble material is removed by extraction with chloroform. The aqueous layer is made acid with acetic acid, and the crystalline precipitate is collected and recrystallized from aqueous dioxane to give 11 g of 2-(5-oxo-5H-[1]benzopyrano[2,3-b]pyridin-7-yl)propionic acid as white needles melting at 194°-195°C.
WORKUP
后处理
- temperatureis heated
- temperatureunder reflux for 24 hours
- concentrationAfter concentration, water
- additionis added to the residue
- additionfurther a 10% sodium hydroxide solution is added
- dissolutionto dissolve the residue
- customAn insoluble material is removed by extraction with chloroform
- customthe crystalline precipitate is collected
- customrecrystallized from aqueous dioxane