反应详情

To a mixture of 1.47 g (2.4 mmol) of 4-ethoxycarbonylbenzoic acid, 3 drops of DMF and 10 ml of benzene is added 0.52 g (4.4 mmol) of thionyl chloride, and the resultant mixture is refluxed for 3 hours under stirring and concentrated in vacuo to dryness. The residue is dissolved in acetone and mixed with 1.4 g of solid potassium carbonate and then 0.5 g (2 mmol) of 3ethoxycarbonyl-9-mercapto-4H-pyrido[1,2-a]pyrimidin-4-one II-1, and the resultant mixture is vigorously stirred at room temperature for 20 minutes. The reaction mixture is concentrated in vacuo to dryness, and the residue is distributed in chloroformwater. The organic layer is dried over sodium sulfate and concentrated in vacuo. The residue is chromatographed on a column of silica gel, which is eluted with ethyl acetate to give 0.9 g of the titled compound Ie-56.

1. concentrationconcentrated in vacuo to dryness
2. dissolutionThe residue is dissolved in acetone
3. additionmixed with 1.4 g of solid potassium carbonate
4. concentrationThe reaction mixture is concentrated in vacuo to dryness
5. dry with materialThe organic layer is dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue is chromatographed on a column of silica gel, which
8. washis eluted with ethyl acetate