反应详情

温度

40 °C

To toluene (810 l) was charged sodium tert-pentoxide (91 kg, 2.3 eq). The mixture was heated to 40° C. and tert-butyl acetoacetate (124.3 kg, 2.2 eq) added. The mixture was heated to 70° C. and trifluoronitrobenzene (63.1 kg, 1.0 eq) added. The temperature was maintained at 70° C. for 3 hours. The mixture was cooled to 25° C. and 20% w/w sulphuric acid added to adjust the pH to 5. The lower aqueous layer was discarded and the organic layer washed twice with water (2×227 kg of water), with 2.3% w/w sodium bicarbonate (192 kg) and then water (192 kg). The organic layer was distilled under vacuum (50 mbar), removing 574 kg of distillate leaving a solution of tert-butyl 2-(2,3-difluoro-6-nitrophenyl)-3-oxobutanoate in toluene.

1. temperatureThe mixture was heated to 70° C.
2. temperatureThe temperature was maintained at 70° C. for 3 hours
3. temperatureThe mixture was cooled to 25° C.
4. washthe organic layer washed twice with water (2×227 kg of water), with 2.3% w/w sodium bicarbonate (192 kg)
5. distillationThe organic layer was distilled under vacuum (50 mbar)
6. customremoving 574 kg