HRID860766

反应详情

EQUATION

反应方程式

HRID 860766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
78 °C

PROCEDURE

实验过程

The reaction is carried out, under nitrogen, in a 1 L×4 neck flask equipped with a mechanical stirrer, water condenser (with gas inlet), and a thermocouple. The reactor is charged with 5-methylpyrazinecarboxylic acid (100 g), ethanol (300 g) and sulfuric acid (2 g). The contents are refluxed for eight hours at 78° C. The reaction mixture is cooled to ambient temperature and sodium bicarbonate (4 g) is added. About 75% of the solvent is removed under reduced pressure and the resulting suspension is allowed to stand overnight. The solids are filtered and washed with cold methanol (2×80 g). Drying under oven (25 inches of Hg) yielded 101.25 g (84%) of 5-methyl-2-pyrazinecarboxylic acid, ethyl ester.

WORKUP

后处理

  1. customequipped with a mechanical stirrer, water condenser (with gas inlet)
  2. temperatureThe reaction mixture is cooled to ambient temperature
  3. customAbout 75% of the solvent is removed under reduced pressure
  4. filtrationThe solids are filtered
  5. washwashed with cold methanol (2×80 g)
  6. customDrying under oven (25 inches of Hg)