تفاعل #792157

معادلة التفاعل

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

المردود 87.3%

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

المردود 87.3%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONthe suspension thinned during the addition
2. 2
   درجة الحرارةThe reaction mixture was then warmed
3. 3
   درجة الحرارةto reflux for 1.5 h
4. 4
   أخرىA new suspension formed
5. 5
   أخرىThe solids were collected
6. 6
   غسيلwashed with ether
7. 7
   أخرىThe solids were air-dried
8. 8
   أخرىdried in vacuo at 90° C. for 5 h

الإجراء التجريبي

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.

المصدر