HRID1650699
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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%).
WORKUP
后处理
- additionwas added dropwise at room temperature under a nitrogen atmosphere
- temperatureThe mixture was refluxed 5 h
- filtrationThe colorless precipitate was collected by filtration
- dissolutiondissolved in 400 ml of water
- extractionAfter basification with ammonia the aqueous solution was extracted with 3×400 ml of dichloromethane
- additionThe combined organic phases were treated with charcoal
- dry with materialdried over magnesium sulphate
- customRemoval of the solvent in vacuo
- customgave a colorless solid, 73