HRID2307995

反应详情

EQUATION

反应方程式

HRID 2307995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 monohydrate 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

  1. temperaturewas heated
  2. temperatureat reflux
  3. customfor 24 hours
  4. temperatureThe mixture was heated
  5. temperatureat reflux overnight
  6. customThe mixture was quenched with water, sat. NaHCO3
  7. extractionextracted with ethyl acetate
  8. customThe organic layer was separated
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated to dryness
  11. customAfter purification