HRID968019
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 4-(1-ethyl-propoxy)-6-methyl-N2-(2,4,6-trimethyl-phenyl)-pyridine-2,3-diamine, trimethyl orthoformate, p-toluenesulfonic acid monohyrate in toluene was heated at reflux using Dean-Stark apparatus for 24 hours. The mixture was heated at reflux overnight. The mixture was quenched with water, sat. NaHCO3, extracted with ethyl acetate. The organic layer was separated, dried (MgSO4) and concentrated to dryness. After purification, the title compound was isolated. Anal. For C21H29N3O.¼H2O calc. C, 73.76; H, 8.10; N, 12.29; found: C, 73.22; H, 7.96; N, 12.42.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux
- customfor 24 hours
- temperatureThe mixture was heated
- temperatureat reflux overnight
- customThe mixture was quenched with water, sat. NaHCO3
- extractionextracted with ethyl acetate
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- concentrationconcentrated to dryness
- customAfter purification