반응 #792157

반응 방정식

benzoxazinone

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

isopropylamine

diethyl ether

→

title compound

수율 87.3%

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

수율 87.3%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONthe suspension thinned during the addition
2. 2
   온도The reaction mixture was then warmed
3. 3
   온도to reflux for 1.5 h
4. 4
   기타A new suspension formed
5. 5
   기타The solids were collected
6. 6
   세척washed with ether
7. 7
   기타The solids were air-dried
8. 8
   기타dried in vacuo at 90° C. for 5 h

실험 절차

To a suspension of the benzoxazinone product of Step D (124 g, 300 mmol) in dichloromethane (500 mL) was added dropwise isopropylamine (76 mL, 900 mmol) at room temperature. The temperature of the reaction mixture rose and the suspension thinned during the addition. The reaction mixture was then warmed to reflux for 1.5 h. A new suspension formed. The reaction mixture was cooled to room temperature and diethyl ether (1.3 L) was added and the mixture stirred at room temperature overnight. The solids were collected and washed with ether. The solids were air-dried and then dried in vacuo at 90° C. for 5 h to yield 122 g of the title compound, a compound of the present invention, as a fluffy white solid, melting at 194-196° C.

출처