HRID279979
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
- 150 °C
PROCEDURE
实验过程
The product of Example 2 was oxidised using 20% palladium on charcoal in 50 ml of cumene, by heating at 150° C. for 21 hours. After the catalyst was removed and the solvent evaporated, the residue was purified on a silica gel column which was eluted with methylene chloride:methanol/19:1. This produced 0.51 g (35%) of the title compound, which melted at 285°-287° after recrystallisation from betamethoxyethanol. Anal. Calcd. for C15H15N5O: C, 64.04; H, 5.37; N, 24.89. Found: C, 63.88; H, 5.37; N, 24.84.
WORKUP
后处理
- customAfter the catalyst was removed
- customthe solvent evaporated
- customthe residue was purified on a silica gel column which
- washwas eluted with methylene chloride
- customThis produced 0.51 g (35%) of the title compound, which melted at 285°-287° after recrystallisation from betamethoxyethanol