反应详情

To a solution of 0.45 g (0.93 mmol) of 7-[4-(imidazo[1,2-a]pyridin-5-ylthio)butyl]-1,1-dioxo-9-phenyl-3,4-dihydro-2H,6H-pyrimido[6,1-b][1,3]thiazine-6,8(7H)-dione in 10 ml of acetonitrile, 0.258 g (1.4 mmol) of N,N-dimethylmethylene ammonium iodide (Eschenmoser's salt) was added at room temperature, followed by refluxing for 2 hours. After the reaction mixture was cooled, the solvent was distilled off. The residue was dissolved in dichloromethane, washed with saturated aqueous sodium hydrogen carbonate and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent, chloroform/methanol=25/1) to yield 0.40 g (77.6%, light yellow oily substance) of the desired product.

1. temperatureby refluxing for 2 hours
2. temperatureAfter the reaction mixture was cooled
3. distillationthe solvent was distilled off
4. dissolutionThe residue was dissolved in dichloromethane
5. washwashed with saturated aqueous sodium hydrogen carbonate
6. customdried
7. distillationafter which the solvent was distilled off
8. customThe residue was purified by column chromatography (eluent, chloroform/methanol=25/1)