HRID909533

反应详情

EQUATION

反应方程式

HRID 909533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Commercially available 5-hydroxypyrazine-2-carboxylic acid (1.00 g, 7.14 mmol) was dissolved in methanol (5 mL), and a 4N hydrochloric acid/dioxane solution (25 mL) was added, followed by stirring at 60° C. for 1.5 hours and heating to reflux at 80° C. for 2.5 hours. The reaction solution was brought back to room temperature, the solvent was distilled off under reduced pressure, and ethyl acetate (20 mL) was added to the resulting residue to allow it to be suspended. The resulting precipitate was filtered off, and washed with ethyl acetate, followed by vacuum drying, to afford the desired compound (673 mg, yield 61%) as an orange-brown solid.

WORKUP

后处理

  1. temperatureheating
  2. temperatureto reflux at 80° C. for 2.5 hours
  3. customwas brought back to room temperature
  4. distillationthe solvent was distilled off under reduced pressure, and ethyl acetate (20 mL)
  5. additionwas added to the resulting residue
  6. filtrationThe resulting precipitate was filtered off
  7. washwashed with ethyl acetate
  8. customdrying