HRID1793879
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
A mixture of the product of Example 4, 6-(3,5-dimethoxy-phenyl)-8-ethyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-ylideneamine (50.0 g, 0.145 mol), and acetic anhydride (150 mL) were heated with stirring until reflux at which point all the starting material dissolved. The reaction mixture was heated at reflux for 5 minutes, cooled in an ice bath, and t-butyl methyl ether added. The product was collected by filtration, washed with acetic anhydride (50 mL) and ether (100 mL) to afford 43.7 g (78% yield) of the titled compound. mp 145–150° C.
WORKUP
后处理
- temperaturewere heated
- temperatureuntil reflux at which point all the starting material
- dissolutiondissolved
- temperatureThe reaction mixture was heated
- temperatureat reflux for 5 minutes
- temperaturecooled in an ice bath
- filtrationThe product was collected by filtration
- washwashed with acetic anhydride (50 mL) and ether (100 mL)