反応 #792159

反応方程式

benzoxazinone

6-chloro-2-[1-(3-chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazin-4-one

isopropylamine

→

title compound

N-[4-Chloro-2-methyl-6-[[(1-methylethyl)amino]carbonyl]-phenyl]-1-(3-chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度The reaction mixture was then warmed until all solids
2. 2
   workup.DISSOLUTIONhad dissolved
3. 3
   その他The tetrahydrofuran solvent was evaporated under reduced pressure
4. 4
   その他the residual solid was purified by chromatography on silica gel

実験手順

To a solution of the benzoxazinone product of Step D (5.0 g, 11.3 mmol) in tetrahydrofuran (35 mL) was added dropwise isopropylamine (2.9 mL, 34.0 mmol) in tetrahydrofuran (10 mL) at room temperature. The reaction mixture was then warmed until all solids had dissolved and stirred an additional five minutes, at which point thin layer chromatography on silica gel confirmed completion of the reaction. The tetrahydrofuran solvent was evaporated under reduced pressure, and the residual solid was purified by chromatography on silica gel, followed by trituration with ether/hexane to afford the title compound, a compound of the present invention, as a solid (4.6 g), melting at 195-196° C.

出典