HRID1171186
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
2,6-diamino-nicotinic acid ethyl ester (2 g, 11 mmol) described in Production Example 1-1-3 was dissolved in ethanol (15 mL) followed by the addition of 1 N aqueous sodium hydroxide solution (15 mL) and stirring for 2 hours while heating under reflux. After allowing the reaction mixture to return to room temperature, the ethanol was distilled off under a reduced pressure and the residue was cooled with ice and neutralized with 1 N hydrochloric acid. After filtering the precipitated solid and washing with water, the solid was dried to obtain the title compound (1.72 g, 11 mmol, quantitative).
WORKUP
后处理
- temperaturewhile heating
- temperatureunder reflux
- customto return to room temperature
- distillationthe ethanol was distilled off under a reduced pressure
- temperaturethe residue was cooled with ice and neutralized with 1 N hydrochloric acid
- filtrationAfter filtering the precipitated solid
- washwashing with water
- customthe solid was dried