HRID2350859
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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 11.4 g (0.1114 mole) of 1-aminopiperidine was heated at 160° C. for 1 hour. The mixture was concentrated by Kugelrohr distillation and the residue was partitioned between methylene chloride and water. The organic layer was dried (sodium sulfate) and concentrated to a small volume. The resulting crystals were collected to give 5.74 g of 2,10-dihydro-10-(1-piperidinyl)imidazo[1,2-a]pyrido[2,3-d]pyrimidin-5(3H)-one. Melting point 206°-207° C. Total yield 54%.
WORKUP
后处理
- concentrationThe mixture was concentrated by Kugelrohr distillation
- customthe residue was partitioned between methylene chloride and water
- dry with materialThe organic layer was dried (sodium sulfate)
- concentrationconcentrated to a small volume
- customThe resulting crystals were collected