반응 #1933561

반응 방정식

4-methyl-3-nitrobenzaldehyde

2-amino-N-(4-sec-butylphenyl)benzamide

→

3-(4-sec-butylphenyl)-2-(4-methyl-3-nitrophenyl)quinazolin-4(3H)-one

수율 81.0%

용매

EtOH

반응 조건

후처리

1. 1
   온도After heating
2. 2
   온도at reflux temperature for 2 hours
3. 3
   농축the reaction mixture was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in EtOAc
5. 5
   세척washed with H2O
6. 6
   건조brine, dried (Na2SO4)
7. 7
   여과filtered
8. 8
   농축concentrated in vacuo
9. 9
   기타Purification by flash chromatography on silica gel
10. 10
    세척eluting with 5% to 60% EtOAc in heptane

실험 절차

4-methyl-3-nitrobenzaldehyde (0.246 g, 1.50 mmol) and anhydrous CuCl2 (0.400 g, 3.00 mmol) were added to a solution of 2-amino-N-(4-sec-butylphenyl)benzamide (0.400 g, 1.50 mmol) in anhydrous EtOH (15 mL). After heating at reflux temperature for 2 hours, the reaction mixture was concentrated in vacuo. The residue was dissolved in EtOAc, washed with H2O, then brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 5% to 60% EtOAc in heptane, afforded 3-(4-sec-butylphenyl)-2-(4-methyl-3-nitrophenyl)quinazolin-4(3H)-one (0.500 g, 81%).

출처