HRID1898789

反应详情

EQUATION

反应方程式

HRID 1898789 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washwashed in with 6.5 ml of ethanol
  2. temperatureto reflux
  3. additiondiluted with a further 30 ml of water
  4. temperaturecooled again
  5. temperatureafter heating for 1 hour
  6. additionafter the addition of 500 ml of acetone
  7. filtrationwas filtered off with suction
  8. washwashed
  9. customdried