HRID619698
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
45 g (0.168 mol) of diethyl 5-nitropyridine-2,3-dicarboxylate were added in the course of 10 minutes with stirring to a mixture of 13.4 g (0.336 mol) of sodium hydroxide in 65 ml of water and washed in with 6.5 ml of ethanol. The mixture was brought to reflux, diluted with a further 30 ml of water and cooled again after heating for 1 hour. The precipitate deposited after the addition of 500 ml of acetone was filtered off with suction, washed and dried, 42.4 g (98.6% of theory) of sodium 5-nitropyridine-2,3-dicarboxylate of m.p. >260° C. being obtained.
WORKUP
后处理
- washwashed in with 6.5 ml of ethanol
- temperatureto reflux
- additiondiluted with a further 30 ml of water
- temperaturecooled again
- temperatureafter heating for 1 hour
- additionafter the addition of 500 ml of acetone
- filtrationwas filtered off with suction
- washwashed
- customdried