反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated for 2 hours
- temperatureunder reflux
- temperatureheating
- temperatureunder reflux
- temperatureto cool off
- concentrationconcentrated under reduced pressure, 10 mL of water
- additionwas added
- extractionextracted with 60 mL of ethyl acetate
- washThe organic layer was washed with 10 mL of saturated saline solution
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customthe residue was purified on silica gel chromatography (hexane:ethyl acetate=2:1)