HRID1171186

反应详情

EQUATION

反应方程式

HRID 1171186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewhile heating
  2. temperatureunder reflux
  3. customto return to room temperature
  4. distillationthe ethanol was distilled off under a reduced pressure
  5. temperaturethe residue was cooled with ice and neutralized with 1 N hydrochloric acid
  6. filtrationAfter filtering the precipitated solid
  7. washwashing with water
  8. customthe solid was dried