反应详情

To a solution of 4.98 g (25 mmol) of 4-amino-2-(4-hydroxybutylthio)pyrimidine in 70 ml of ethanol, 30 ml of a 40% chloroacetaldehyde solution was added, followed by refluxing for 4 hours. After the reaction mixture was cooled, the solvent was distilled off. The residue was dissolved in chloroform, washed with saturated aqueous sodium hydrogen carbonate and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent, n-hexane/ethyl acetate=1/1→1/4→ethyl acetate) to yield 3.15 g (56.4%, white crystal) of the desired product.

1. temperatureby refluxing for 4 hours
2. temperatureAfter the reaction mixture was cooled
3. distillationthe solvent was distilled off
4. dissolutionThe residue was dissolved in chloroform
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, n-hexane/ethyl acetate=1/1→1/4→ethyl acetate)