反应详情

To a suspension of 2-[1-(3-chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazin-4-one (the product from 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 the dried in vacuo at 90° C. for 5 h to yield 122 g of the title compound as a fluffy white solid, melting at 194–196° C.

1. additionthe suspension thinned during the addition
2. temperatureThe reaction mixture was then warmed
3. temperatureto reflux for 1.5 h
4. customA new suspension formed
5. customThe solids were collected
6. washwashed with ether
7. customThe solids were air-dried
8. customthe dried in vacuo at 90° C. for 5 h