反应详情

16.4 g (0.12 mol) of isobutyl chloroformate are added dropwise to a mixture of 8.3 g (0.05 mol) of 2,4-diamino-6-cyclopropylamino-s-triazine, 0.5 g of 4-dimethylaminopyridine and 125 ml of pyridine. The batch is stirred for 1 hour at room temperature and then for 1 hour at 55°-60° C. After the precipitate has been filtered off, the reaction mixture is concentrated by evaporation in a water-jet vacuum, the residue is taken up in 150 ml of chloroform and extracted with 100 ml of water. After drying over sodium sulfate, the solvent is distilled off, and the crude product is purified by column chromatography through silica with methylene chloride as eluant.

1. waitfor 1 hour at 55°-60° C
2. filtrationAfter the precipitate has been filtered off
3. concentrationthe reaction mixture is concentrated by evaporation in a water-jet vacuum
4. extractionextracted with 100 ml of water
5. dry with materialAfter drying over sodium sulfate
6. distillationthe solvent is distilled off
7. customthe crude product is purified by column chromatography through silica with methylene chloride as eluant