反应详情

2-(2-Fluorophenyl)-1,5-dimethyl-1H-pyrazol-3(2H)-one (260 g, 1261 mmol) in TFA (1040 ml) was cooled to −10° C. and stirred for 30 mins. To the mixture was added fuming nitric acid (84 ml) dropwise and this was stirred for 15 mins under cooling then at RT for 1 hr. The resulting mixture was poured onto a mixture of ice (1500 ml), water (1000 ml) and TBME (2500 ml) and stirred until the ice melted, then at RT for 1 hr. The mixture was filtered, washed with water (200 ml) and TBME (1000 ml). The collected crystals were dried to give the title compound as red-brown crystals.

1. stirringthis was stirred for 15 mins
2. temperatureunder cooling
3. waitat RT for 1 hr
4. waitat RT for 1 hr
5. filtrationThe mixture was filtered
6. washwashed with water (200 ml) and TBME (1000 ml)
7. customThe collected crystals were dried