HRID2350860

反应详情

EQUATION

反应方程式

HRID 2350860 的结构方程式

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 10.0 g (39.1 mmoles) of the product of Example 12 and 12.5 g (0.109 mole) of N-aminohomopiperidine was heated at 160° C. for 1 hour. Excess N-aminohomopiperidine was removed by Kugelrohr distillation and the residue was partitioned between methylene chloride and water. The organic layer was dried (sodium sulfate) and concentrated leaving 7.40 g of 10-(hexahydro-1H-azepin-1yl)-2,10-dihydroimidazo[1,2-a]pyrido[2,3-d]pyrimidin-5(3H)-one; melting point 217°-219° C. Total yield 66%.

WORKUP

后处理

  1. customExcess N-aminohomopiperidine was removed by Kugelrohr distillation
  2. customthe residue was partitioned between methylene chloride and water
  3. dry with materialThe organic layer was dried (sodium sulfate)
  4. concentrationconcentrated