HRID1511823

反应详情

EQUATION

反应方程式

HRID 1511823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100 mg of 3-phenylpyrido[2,3-b]pyrazin-6-ylamine (0.45 mmol) were dissolved in pyridine and admixed with 191 mg of p-nitrophenyl N-methoxycarbamate (0.90 mmol). The mixture was heated under reflux for 4 h. For workup, the pyridine was removed under reduced pressure, and the residue was partitioned in ethyl acetate and distilled water. The phases were separated and the aqueous phase was extracted twice with ethyl acetate. The combined organic phases were dried over MgSO4 and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (dichloromethane/methanol eluent). A light beige solid was isolated.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 h
  3. customFor workup, the pyridine was removed under reduced pressure
  4. customthe residue was partitioned in ethyl acetate
  5. distillationdistilled water
  6. customThe phases were separated
  7. extractionthe aqueous phase was extracted twice with ethyl acetate
  8. dry with materialThe combined organic phases were dried over MgSO4
  9. customthe solvent was removed under reduced pressure
  10. customThe residue was purified by column chromatography on silica gel (dichloromethane/methanol eluent)
  11. customA light beige solid was isolated