Reaktion #1687628

Reaktionsgleichung

aminoacetone

nicotinoyl chloride

→

N-Acetylmethyl-nicotinamide

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added dropwise at room temperature under a nitrogen atmosphere
2. 2
   TemperaturThe mixture was refluxed 5 h
3. 3
   FiltrationThe colorless precipitate was collected by filtration
4. 4
   workup.DISSOLUTIONdissolved in 400 ml of water
5. 5
   ExtraktionAfter 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
   Trocknendried over magnesium sulphate
8. 8
   SonstigeRemoval of the solvent in vacuo
9. 9
   Sonstigegave a colorless solid, 73

Vorschrift

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%).

Quelle