反应详情

温度

76 °C

Into a 100-mL 3-necked round-bottom flask, was placed a solution of 2-amino-4-bromo-N′-phenylbenzohydrazide (4 g, 13.07 mmol, 1.00 equiv) in 1N HCl:Ethanol=1:1 (40 mL). The resulting solution was heated to 76° C. The solid dissolved to yield red solution. To the resulting mixture was then added a solution of NaNO2 (2.7 g, 39.13 mmol, 3.00 equiv) in water (5 mL) dropwise with stirring at 76° C. The resulting solution was stirred for 1 h at 76° C. in an oil bath. The resulting mixture was cooled to 20° C. with a water bath. The solids were collected by filtration, washed with water (2×40 mL), then dried in an oven under reduced pressure to yield 6-bromo-1-phenyl-1,2-dihydroindazol-3-one as a red solid. MS: 288 (MH+).

1. customInto a 100-mL 3-necked round-bottom flask, was placed
2. dissolutionThe solid dissolved
3. customto yield red solution
4. stirringThe resulting solution was stirred for 1 h at 76° C. in an oil bath
5. temperatureThe resulting mixture was cooled to 20° C. with a water bath
6. filtrationThe solids were collected by filtration
7. washwashed with water (2×40 mL)
8. customdried in an oven under reduced pressure