HRID326822

反应详情

EQUATION

反应方程式

HRID 326822 的结构方程式

PROCEDURE

实验过程

A mixture of 8.3 g (0.060 mole) of 3-amino-2-pyrazinecarboxamide [prepared according to R. C. Ellingson et al., J. Am. Chem. Soc. 1945, 67, 1711], 49.5 g (0.24 mole) of triethyl orthoethoxyacetate [prepared according to S. M. McElvain and P. M. Walters, J. Am. Chem. Soc. 1942, 64, 1963] and 53 ml of acetic anhydride is refluxed under a nitrogen atmosphere for 3 hours. The temperature of this reflux falls with the passage of time from 124° to 96° C. and then remains constant at the latter temperature. After cooling, the precipitate formed is isolated by filtration. It is washed with ether and recrystallized from ethanol. Yld: 5.5 g (44%), m.p. 168°-169° C.

WORKUP

后处理

  1. temperatureis refluxed under a nitrogen atmosphere for 3 hours
  2. customfalls with the passage of time from 124° to 96° C.
  3. temperatureAfter cooling
  4. customthe precipitate formed
  5. customis isolated by filtration
  6. washIt is washed with ether
  7. customrecrystallized from ethanol