HRID463361

反应详情

EQUATION

反应方程式

HRID 463361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 20 mL of water and 8.40 g (0.105 mol) of 50% sodium hydroxide solution is added 7.83 g (0.030 mol) of 2-[(1-cyano-1,2-dimethylpropyl)aminocarbonyl]nicotinic acid. External heating is applied to raise the temperature to 70°-75° C. where it is maintained for five hours. After cooling the reaction mixture to 20°-30° C., 50 mL of methylene chloride is added and the pH is adjusted to 3.0 by the addition of 37% hydrochloric acid. The organic layer is separated and the solvent is removed by distillation to give 6.71 g of solid 2-(5-isopropyl-5-methyl-4-oxo-2-imidazolin-2-yl)nicotinic acid which is 90% pure in 77% yields.

WORKUP

后处理

  1. temperatureExternal heating
  2. temperatureto raise the temperature to 70°-75° C. where it
  3. temperatureis maintained for five hours
  4. temperatureAfter cooling the reaction mixture to 20°-30° C.
  5. customThe organic layer is separated
  6. customthe solvent is removed by distillation