HRID422039

反应详情

EQUATION

反应方程式

HRID 422039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 160 mg of methyl 2-(3-chlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate which was synthesized in Production Example 1, 65 mg of potassium carbonate, 20 mL of acetonitrile and 67 mg of methyl iodide was heated for 2 hours under reflux. Further 20 mg of methyl iodide was added, followed by another hour's heating under reflux. The reaction mixture was allowed to cool off, and then concentrated under reduced pressure, 10 mL of water was added thereto, and extracted with 60 mL of ethyl acetate. The organic layer was washed with 10 mL of saturated saline solution, dried over magnesium sulfate, concentrated under reduced pressure, and the residue was purified on silica gel chromatography (hexane:ethyl acetate=2:1) to provide 130 mg of the title compound.

WORKUP

后处理

  1. temperaturewas heated for 2 hours
  2. temperatureunder reflux
  3. temperatureheating
  4. temperatureunder reflux
  5. temperatureto cool off
  6. concentrationconcentrated under reduced pressure, 10 mL of water
  7. additionwas added
  8. extractionextracted with 60 mL of ethyl acetate
  9. washThe organic layer was washed with 10 mL of saturated saline solution
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated under reduced pressure
  12. customthe residue was purified on silica gel chromatography (hexane:ethyl acetate=2:1)