反応 #792157

反応方程式

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

収率 87.3%

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

収率 87.3%

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONthe suspension thinned during the addition
2. 2
   温度The reaction mixture was then warmed
3. 3
   温度to reflux for 1.5 h
4. 4
   その他A new suspension formed
5. 5
   その他The solids were collected
6. 6
   洗浄washed with ether
7. 7
   その他The solids were air-dried
8. 8
   その他dried in vacuo at 90° C. for 5 h

実験手順

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.

出典