反应详情

13.9 g of 7-nitro-1(2H)-phthalazinone and 16.3 g of Lawesson reagent in 170 ml of acetonitrile are heated under reflux for 45 minutes. The reaction mixture is filtered while hot. The filtrate is cooled in an ice-bath and the crystals obtained are removed by filtration under suction. After drying in vacuo and recrystallization there is obtained 7-nitro-1(2H)-phthalazinethione as yellow crystals of m.p. 233+-234° (methanol/acetonitrile).

1. temperatureunder reflux for 45 minutes
2. filtrationThe reaction mixture is filtered while hot
3. temperatureThe filtrate is cooled in an ice-bath
4. customthe crystals obtained
5. customare removed by filtration under suction
6. customAfter drying in vacuo
7. customrecrystallization there