반응 #678991

반응 방정식

2,6-dimethyl-pyridine-4-carbaldehyde

2-amino-4,6-difluorobenzamide

sodium hydrogen sulfite

p-toluenesulfonic acid

→

2-(2,6-dimethyl-pyridin-4-yl)-5,7-difluoro-3H-quinazolin-4-one

용매

N,N-dimethyl acetamide

반응 조건

후처리

1. 1
   온도After cooling to room temperature
2. 2
   기타the solvent was evaporated under reduced pressure
3. 3
   workup.ADDITIONWater (50 mL) was added
4. 4
   여과the precipitated solid was filtered
5. 5
   세척washed with water
6. 6
   기타dried under vacuum

실험 절차

To a solution of 2,6-dimethyl-pyridine-4-carbaldehyde (0.99 g, 7.32 mmol) and 2-amino-4,6-difluorobenzamide (1.26 g, 7.32 mmol) in N,N-dimethyl acetamide (20 mL) were added sodium hydrogen sulfite (58.5 wt %, 1.59 g, 8.78 mmol) and p-toluenesulfonic acid (0.21 g, 1.09 mmol). The reaction mixture was stirred at 115° C. for 16 hours under nitrogen. After cooling to room temperature, the solvent was evaporated under reduced pressure. Water (50 mL) was added, the precipitated solid was filtered, washed with water, and dried under vacuum, to give 2-(2,6-dimethyl-pyridin-4-yl)-5,7-difluoro-3H-quinazolin-4-one as a yellow solid. Yield: 0.63 g (30%).

출처