反応 #1687628

反応方程式

aminoacetone

nicotinoyl chloride

→

N-Acetylmethyl-nicotinamide

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise at room temperature under a nitrogen atmosphere
2. 2
   温度The mixture was refluxed 5 h
3. 3
   ろ過The colorless precipitate was collected by filtration
4. 4
   workup.DISSOLUTIONdissolved in 400 ml of water
5. 5
   抽出After 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
   乾燥dried over magnesium sulphate
8. 8
   その他Removal of the solvent in vacuo
9. 9
   その他gave a colorless solid, 73

実験手順

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%).

出典