HRID1270423

反应详情

EQUATION

反应方程式

HRID 1270423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.5 g (12.7 mmol) of 2-[(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-amino]-benzoic acid-methyl ester is mixed in 15 ml of dimethylformamide with 30 ml of 6N sodium hydroxide solution and stirred for 1.5 hours at room temperature. While being cooled with ice, it is then mixed with about 50 ml of 4N hydrochloric acid, the precipitation is suctioned off, and it is washed with water. 3.1 g, which is taken up in 29.3 ml of 1N sodium hydroxide solution and 142 ml of ethanol, is obtained, and it is heated for 1.5 hours to a bath temperature of 120° C. The ethanol is then drawn off in a vacuum, it is made acidic with 2N hydrochloric acid, and the precipitated product is suctioned off and dried well. 2.9 g (93.5% of theory) of 2-[(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-amino]-benzoic acid is obtained.

WORKUP

后处理

  1. temperatureWhile being cooled with ice, it
  2. customthe precipitation
  3. washit is washed with water
  4. custom142 ml of ethanol, is obtained
  5. temperatureit is heated for 1.5 hours to a bath temperature of 120° C
  6. customdried well