반응 #679017

반응 방정식

2-amino-4,6-difluoro-benzamide

2-methyl-pyridine-4-carbaldehyde

NaHSO3

p-TSA

→

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

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   기타The solvent was removed under reduced pressure
3. 3
   기타The crude compound was purified by column chromatography (silica gel 230-400 mesh; 5% methanol in dichloromethane)

실험 절차

To a solution of 2-amino-4,6-difluoro-benzamide (0.71 g, 4.10 mmol) and 2-methyl-pyridine-4-carbaldehyde (0.50 g, 4.10 mmol) in N,N-dimethylacetamide (10 mL) were added NaHSO3 (58.5 wt %, 1.00 g, 5.70 mmol) and p-TSA (0.16 g, 0.08 mmol). The reaction mixture was heated at 115° C. for 30 hours, then cooled to room temperature. The solvent was removed under reduced pressure. The crude compound was purified by column chromatography (silica gel 230-400 mesh; 5% methanol in dichloromethane) to afford 5,7-difluoro-2-(2-methyl-pyridin-4-yl)-3H-quinazolin-4-one as a light yellow solid. Yield: 0.30 g (26%).

출처