反应 #792157

反应方程式

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

收率 87.3%

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

收率 87.3%

溶剂

dichloromethane

反应条件

后处理

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
   其他A new suspension formed
5. 5
   其他The solids were collected
6. 6
   洗涤washed with ether
7. 7
   其他The solids were air-dried
8. 8
   其他dried in vacuo at 90° C. for 5 h

实验过程

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.

来源