HRID2079948

反应详情

EQUATION

反应方程式

HRID 2079948 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 described in Preparation Example A-14 (2 g, 11 mmol) was dissolved in ethanol (15 mL), an aqueous solution of 1N sodium hydroxide (15 mL) was added thereto, followed by stirring for 2 hours under reflux. The reaction solution was allowed to room temperature, ethanol was then removed by evaporation, the residue was cooled on an ice bath, then neutralized with 1N hydrochloric acid. The precipitated solid was collected by filtration, washed with water, then, dried to obtain the title compound (1.72 g, 11 mmol, quantitatively).

WORKUP

后处理

  1. temperatureunder reflux
  2. customwas allowed to room temperature
  3. customethanol was then removed by evaporation
  4. temperaturethe residue was cooled on an ice bath
  5. filtrationThe precipitated solid was collected by filtration
  6. washwashed with water
  7. customdried