反应详情

A 22 liter (L), 3-necked round-bottom flask with a bottom outlet was fitted with a mechanical stirrer, a condenser topped with a nitrogen inlet, and an addition funnel. Through the funnel, 6.546 kilograms (kg) (33.13 moles) of molten methyl 2-(4-hydroxyphenoxy)propionate, 6.571 kg (47.55 moles) of anhydrous K2CO3 and 319 g (0.99 moles) of tetra-n-butylammonium bromide were added to the reactor. Under constant agitation, the slurry was heated to 66° C. with a steam-water mixture controlled by a microprocessor and 6.026 kg (32.93 moles) of 2,3-difluoro-5-trifluoromethyl-pyridine was added over 15 min. The reaction mixture was heated for 13 hours (hr) at 70°-75° C. after which the product was washed 5 times using a total 37 L of hot water. The washed product was stripped of residual water using a rotary evaporator at 75° C. at a reduced pressure of 30 millimeters (mm) of mercury. A total 10.7 kg of product was collected having a purity of 97.9 percent.

1. customtopped with a nitrogen inlet, and an addition funnel
2. additionwas added over 15 min
3. temperatureThe reaction mixture was heated for 13 hours (hr) at 70°-75° C. after which the product
4. washwas washed 5 times
5. customa rotary evaporator at 75° C. at a reduced pressure of 30 millimeters (mm) of mercury
6. customA total 10.7 kg of product was collected