반응 #1687628

반응 방정식

aminoacetone

nicotinoyl chloride

→

N-Acetylmethyl-nicotinamide

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise at room temperature under a nitrogen atmosphere
2. 2
   온도The mixture was refluxed 5 h
3. 3
   여과The colorless precipitate was collected by filtration
4. 4
   workup.DISSOLUTIONdissolved in 400 ml of water
5. 5
   추출After basification with ammonia the aqueous solution was extracted with 3×400 ml of dichloromethane
6. 6
   workup.ADDITIONThe combined organic phases were treated with charcoal
7. 7
   건조dried over magnesium sulphate
8. 8
   기타Removal of the solvent in vacuo
9. 9
   기타gave a colorless solid, 73

실험 절차

To a suspension of 40 g (0.370 mol) of aminoacetone in 500 ml of dry dichloromethane, 50 g (0.350 mol) of nicotinoyl chloride was added dropwise at room temperature under a nitrogen atmosphere. The mixture was refluxed 5 h followed by stirring overnight at room temperature. The colorless precipitate was collected by filtration and dissolved in 400 ml of water. After basification with ammonia the aqueous solution was extracted with 3×400 ml of dichloromethane. The combined organic phases were treated with charcoal and dried over magnesium sulphate. Removal of the solvent in vacuo gave a colorless solid, 73. Yield: 30.0 g (0.170 mol, 48%).

출처