反应详情

温度

100 °C

18.25 g of hydrazine sulfate and 14.88 g of sodium carbonate are stirred in 300 ml of DMF at 100° C. for one hour. Then, 7.24 g of 3-bromo-4-nitro-phthalide in 100 ml of DMF is added, and it is stirred for another 4 hours at 100° C. It is added to water, extracted several times with ethyl acetate, and the organic phase is washed with water and brine. It is dried, and the solvent is removed in a vacuum. After recrystallization from ethyl acetate, 2.35 g of 5-nitro-phthalazin-1-one is obtained as a solid.

1. extractionextracted several times with ethyl acetate
2. washthe organic phase is washed with water and brine
3. customIt is dried
4. customthe solvent is removed in a vacuum
5. customAfter recrystallization from ethyl acetate