HRID1287234

反应详情

EQUATION

反应方程式

HRID 1287234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13.3 g. of 5,6-Diamino-4-butylamino-2-methylpyridine-3-carboxylic acid, ethyl ester (0.05 Mol.) of Example 1 d and 4g. of glyoxal monohydrate, dissolved in 100 ml. of toluene, are refluxed, while the water formed is removed by means of a water separator. After about 3 hours, the reaction is complete and the solution is concentrated. The remaining oily residue is extracted twice with 50 ml. portions of gasoline and addition of activated charcoal. The gasoline extracts are cooled and the crystalline 8-butylamino-6-methylpyrido[2,3-b]pyrazine-7-carboxylic acid, ethyl ester is filtered off, yield 70%; m.p. 56°-58°.

WORKUP

后处理

  1. customformed
  2. customis removed by means of a water separator
  3. concentrationthe solution is concentrated
  4. extractionThe remaining oily residue is extracted twice with 50 ml
  5. additionportions of gasoline and addition of activated charcoal
  6. temperatureThe gasoline extracts are cooled
  7. filtrationthe crystalline 8-butylamino-6-methylpyrido[2,3-b]pyrazine-7-carboxylic acid, ethyl ester is filtered off