반응 #679007

반응 방정식

2-amino-4,6-difluoro-benzamide

2,6-dimethyl-pyridine-4-carbaldehyde

sodium hydrogen sulfite

p-toluenesulfonic acid monohydrate

→

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

용매

N,N-dimethyl acetamide

반응 조건

후처리

1. 1
   기타The solvent was evaporated in vacuo, water
2. 2
   workup.ADDITIONwas added
3. 3
   여과the precipitated solid was filtered

실험 절차

To a stirred solution of 2-amino-4,6-difluoro-benzamide (4.00 g, 0.0237 mol) and 2,6-dimethyl-pyridine-4-carbaldehyde (3.20 g, 0.0237 mol) in N,N-dimethyl acetamide (15 mL), sodium hydrogen sulfite (58.5 wt %, 5.05 g, 0.0284 mol) and p-toluenesulfonic acid monohydrate (0.90 g, 4.74 mmol) were added and the reaction mixture was stirred at 130° C. for 16 hours. The solvent was evaporated in vacuo, water was added, and the precipitated solid was filtered to give 2-(2,6-dimethyl-pyridin-4-yl)-5,7-difluoro-3H-quinazolin-4-one as a yellow solid, which was used in the next step without further purifications. Yield: 3.70 g (42%).

출처