반응 #603702

반응 방정식

benzoxazinone

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

methylamine

→

title compound

3-Bromo-N-[4-chloro-2-methyl-6-[(methylamino)carbonyl]phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxamide

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   기타The tetrahydrofuran solvent was evaporated under reduced pressure
3. 3
   기타the residual solid was triturated with ether
4. 4
   여과filtered
5. 5
   기타dried

실험 절차

To a solution of the benzoxazinone product of Example 10, Step E (0.20 g, 0.44 mmol) in tetrahydrofuran was added methylamine (2.0 M solution in THF, 0.514 mL, 1.02 mmol), and the reaction mixture was heated to 60° C. for 90 minutes and then cooled to room temperature. The tetrahydrofuran solvent was evaporated under reduced pressure, and the residual solid was triturated with ether, filtered, and dried to afford the title compound, a compound of the present invention, as a solid (40 mg), m.p. 162-164° C.

출처