反应详情

温度

7 °C

In a 10 L-reaction flask, 594 g (1.92 mol) of 3-oxo-2-(4-tert-butylphenyl)-3-(1,3,4-trimethylpyrazol-5-yl)propionitrile and 6000 g of tetrahydrofuran were added, 214 g (2.11 mol) of triethyl amine was added and then 255 g (2.11 mol) of pivaloyl chloride was added dropwise at 25 to 27° C. over 1 hour. After reacting for 20 hours, tetrahydrofuran was removed by concentrating under a reduced pressure, and then 1800 g of toluene and 1800 g of water were added to separate out toluene phase. After distilling out toluene, 794 g of hexane was added and dissolved, and crystallization was carried out by gradually cooling to 7° C. After filtering, the crystal was washed with 1000 g of hexane cooled at 5° C., dried to obtain 554 g (yield 73.4%) of (2E)-3-(2,2-dimethylpropanoyloxy)-2-(4-tert-butylphenyl)-3-(1,3,4-trimethylpyrazol-5-yl)acrylonitrile.

1. additionwere added
2. customtetrahydrofuran was removed
3. concentrationby concentrating under a reduced pressure
4. addition1800 g of toluene and 1800 g of water were added
5. customto separate out toluene phase
6. distillationAfter distilling out toluene, 794 g of hexane
7. additionwas added
8. dissolutiondissolved
9. customcrystallization
10. filtrationAfter filtering
11. washthe crystal was washed with 1000 g of hexane
12. temperaturecooled at 5° C.
13. customdried