反应详情

In a nitrogen atmosphere, 28.6 ml (200 mmol) of ethyl 4-bromobutyrate was added to a solution of 25.44 g (200 mmol) of 2-thiocytosine and 30.7 ml (220 mmol) of triethylamine in 400 ml of ethanol at room temperature, followed by refluxing for 16 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=1/4→1/9) to yield 46.31 g (96.0%, white crystal) of the desired product.

1. temperatureby refluxing for 16 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=1/4→1/9)