HRID2090556

反应详情

EQUATION

反应方程式

HRID 2090556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Combine 2-amino-5-fluoro-4-chloro-1-methyl-6-oxo-1,6-dihydropyridine-carbonitrile (4.97 g, 246 mmol) and 99% formic acid (40 mL, 8 volumes) in a dried vessel. Heat to 80° C. When a solution is formed add aqueous 9 N sulfuric acid (25 mL, 5 volumes). After 20 hours, cool ambient temperature and add ice-water (50 mL, 10 volumes) with stirring. Cool in an ice bath to give a solid. After 30 minutes, collect the solid by filtration, rinse with water (2×5 mL), and dry in vacuo to give the title compound.

WORKUP

后处理

  1. customWhen a solution is formed
  2. temperaturecool ambient temperature
  3. temperatureCool in an ice bath
  4. customto give a solid
  5. waitAfter 30 minutes
  6. customcollect the solid
  7. filtrationby filtration
  8. washrinse with water (2×5 mL)
  9. customdry in vacuo