反应详情

温度

23 °C

1-Butyl-3-(2-fluorobenzyl)-6-[2-(4-nitro-phenyl)-ethylamino]-1H-pyrimidine-2,4-dione (2.3 g, 5.2 mmol) was dissolved in ethanol (20 mL) and treated with isoamyl nitrite (Aldrich) (3.6 mL, 26 mmol). Concentrated aqueous hydrochloric acid (1 mL) was added to the reaction mixture. The reaction was stirred at 23° C. for 40 minutes. The ethanol was removed under reduced pressure and the residue washed with diethyl ether. The solid residue was then dissolved in n-butanol (15 mL), and the mixture refluxed for 30 minutes. After cooling to room temperature 1-butyl-3-(2-fluorobenzyl)-6-[2-(4-nitro-phenyl)-ethylamino]-1H-pyrimidine-2,4-dione separated as pale yellow crystals which were collected by filtration (1.91 g, 81%). LCMS, m/z(M+H)=452.24.

1. customThe ethanol was removed under reduced pressure
2. washthe residue washed with diethyl ether
3. dissolutionThe solid residue was then dissolved in n-butanol (15 mL)
4. temperaturethe mixture refluxed for 30 minutes
5. temperatureAfter cooling to room temperature 1-butyl-3-(2-fluorobenzyl)-6-[2-(4-nitro-phenyl)-ethylamino]-1H-pyrimidine-2,4-dione
6. customseparated as pale yellow crystals which
7. filtrationwere collected by filtration (1.91 g, 81%)