反应详情

温度

100 °C

(4-methoxybenzyl)hydrazine hydrochloride (2.132 g, 11.30 mmol) and 3-bromofuran-2,5-dione (2 g, 11.30 mmol) in water (20 ml) was stirred and heated at 100° C. overnight. The mixture was cooled to room temperature and filtered to collect the solid. The solid was triturated with a mixture of ethyl acetate and ethyl ether (1/4) and the mixture was filtered. The insoluble residue was 4-bromo-1-(4-methoxybenzyl)-1,2-dihydropyridazine-3,6-dione. LRMS m/z (M+H) 311.0 found, 311.0 required. The filtrate was concentrated in vacuo and the residue was purified by column chromatography on silica gel (Petroleum ether: ethyl acetate=1/1)) to give 5-bromo-1-(4-methoxybenzyl)-1,2-dihydropyridazine-3,6-dione. LRMS m/z (M+H) 311.0 found, 311.0 required.

1. temperatureThe mixture was cooled to room temperature
2. filtrationfiltered
3. customto collect the solid
4. customThe solid was triturated with a mixture of ethyl acetate and ethyl ether (1/4)
5. filtrationthe mixture was filtered
6. concentrationThe filtrate was concentrated in vacuo
7. customthe residue was purified by column chromatography on silica gel (Petroleum ether: ethyl acetate=1/1))