HRID1600446

反应详情

EQUATION

反应方程式

HRID 1600446 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added dropwise at room temperature under a nitrogen atmosphere
  2. temperatureThe mixture was refluxed 5 h
  3. filtrationThe colorless precipitate was collected by filtration
  4. dissolutiondissolved in 400 ml of water
  5. extractionAfter basification with ammonia the aqueous solution was extracted with 3×400 ml of dichloromethane
  6. additionThe combined organic phases were treated with charcoal
  7. dry with materialdried over magnesium sulphate
  8. customRemoval of the solvent in vacuo
  9. customgave a colorless solid, 73