반응 #1933449

반응 방정식

2-amino-N-(4-sec-butyl-phenyl)-4-fluoro-benzamide

3,5-dimethyl-4-(2-hydroxy-ethoxy)-benzaldehyde

sodium bisulfite

p-toluenesulfonic acid

→

3-(4-sec-butyl-phenyl)-7-fluoro-2-[4-(2-hydroxy-ethoxy)-3,5-dimethyl-phenyl]-2,3-dihydro-1H-quinazolin-4-one

수율 7.4%

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   기타The solvent was evaporated in vacuo and water
2. 2
   workup.ADDITIONwas added to the flask
3. 3
   여과The precipitate was filtered off
4. 4
   세척washed with water
5. 5
   기타The solid was triturated with ether
6. 6
   여과filtered off

실험 절차

A mixture of 2-amino-N-(4-sec-butyl-phenyl)-4-fluoro-benzamide (0.920 g, 3.21 mmol), 3,5-dimethyl-4-(2-hydroxy-ethoxy)-benzaldehyde (0.627 g, 3.21 mmol), sodium bisulfite (0.640 g, 3.53 mmol), and p-toluenesulfonic acid (60 mg, 0.32 mmol) in N,N-dimethylacetamide (20 mL) was heated at 120° C. for 16 hours. The solvent was evaporated in vacuo and water was added to the flask. The precipitate was filtered off and washed with water. The solid was triturated with ether and filtered off to give 3-(4-sec-butyl-phenyl)-7-fluoro-2-[4-(2-hydroxy-ethoxy)-3,5-dimethyl-phenyl]-2,3-dihydro-1H-quinazolin-4-one (P) (0.11 g). The filtrate was evaporated under vacuum to give second crop of (1.02 g). The combined yield: 1.13 g (quantitative).

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