Reacción #1687628

Ecuación de reacción

aminoacetone

nicotinoyl chloride

→

N-Acetylmethyl-nicotinamide

Disolventes

dichloromethane

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added dropwise at room temperature under a nitrogen atmosphere
2. 2
   TemperaturaThe mixture was refluxed 5 h
3. 3
   FiltraciónThe colorless precipitate was collected by filtration
4. 4
   workup.DISSOLUTIONdissolved in 400 ml of water
5. 5
   ExtracciónAfter 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
   Secadodried over magnesium sulphate
8. 8
   OtroRemoval of the solvent in vacuo
9. 9
   Otrogave a colorless solid, 73

Procedimiento

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%).

Fuente