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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
Under a nitrogen gas flow, to a solution of 27.7 g of N-(5-cyano-2,2-dimethyl-1,3-dioxan-5-yl)-8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-3-carboxamide in 280 ml of DMF were added 10.0 g of ammonium chloride and 12.0 g of sodium azide at room temperature, followed by stirring at 120° C. for 2 hours. The reaction mixture was left to be cooled to room temperature, and the insoluble materials were then separated by filtration and washed with DMF. The filtrate was added to water, followed by stirring at room temperature for 2 days. The resulting insoluble materials were separated by filtration and washed with water. The obtained residue was dried under reduced pressure to obtain 29.2 g of 8-[(2,6-difluorobenzyl)oxy]-N-[2,2-dimethyl-5-(2H-tetrazol-5-yl)-1,3-dioxan-5-yl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide.
WORKUP
后处理
- waitThe reaction mixture was left
- temperatureto be cooled to room temperature
- customthe insoluble materials were then separated by filtration
- washwashed with DMF
- additionThe filtrate was added to water
- stirringby stirring at room temperature for 2 days
- customThe resulting insoluble materials were separated by filtration
- washwashed with water
- customThe obtained residue was dried under reduced pressure