反应详情

温度

95 °C

To a sample of the title compound of Example 1, Step C (22.3 g, 0.126 mole), suspended in acetonitrile (100 mL) was added crude 1-(2-chlorophenyl)-3-(trifluoromethyl)-1H-pyrazole-5-carbonyl chloride (43 g). The mixture was diluted with 350 mL of pyridine and heated to approximately 95° C. for a period of 2 hours. The mixture was cooled to 29° C., then was treated with isopropylamine (32.2 mL, 0.38 mole). The reaction mass self-heated to 60° C. and was maintained at about 50° C. for one hour, then stirred overnight. The reaction mixture was poured into 1 L of water and stirred. The resulting solid was collected by filtration and washed with water. The wet cake was taken up in a mixture of dichloromethane and methanol, the water removed, and the organic phase was dried with molecular sieves and filtered. Volatiles were removed on a rotary evaporator. The crude product was triturated with 1:1 ether/hexane, collected by filtration and washed with hexanes to yield 42.6 g of a light tan solid melting at 230–231° C.

1. temperatureThe mixture was cooled to 29° C.
2. temperatureThe reaction mass self-heated to 60° C.
3. temperaturewas maintained at about 50° C. for one hour
4. stirringstirred
5. filtrationThe resulting solid was collected by filtration
6. washwashed with water
7. additionThe wet cake was taken up in a mixture of dichloromethane and methanol
8. customthe water removed
9. customthe organic phase was dried with molecular sieves
10. filtrationfiltered
11. customVolatiles were removed on a rotary evaporator
12. customThe crude product was triturated with 1:1 ether/hexane
13. filtrationcollected by filtration
14. washwashed with hexanes