HRID636313

反应详情

EQUATION

反应方程式

HRID 636313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was synthesized via modification of Acta Chem. Scand. B42, 373, 1988. A mixture of NaBH4 (6.8 g, 180 mmol), diethyl 4-bromopyridine-2,6-dicarboxylate (12.1 g, 40 mmol) in absolute EtOH (500 mL) was heated under reflux for 18 h. The solvent was removed in vacuo and the residue was treated with hot saturated aqueous NaHCO3. The mixture was extracted with EtOAc, the combined organic phase was dried (Na2SO4) and evaporated. The dried material was recrystallized from EtOAc to give 7.3 g (83%) of the title compound as white crystals.

WORKUP

后处理

  1. customThe title compound was synthesized via modification of Acta Chem
  2. temperaturewas heated
  3. temperatureunder reflux for 18 h
  4. customThe solvent was removed in vacuo
  5. additionthe residue was treated with hot saturated aqueous NaHCO3
  6. extractionThe mixture was extracted with EtOAc
  7. dry with materialthe combined organic phase was dried (Na2SO4)
  8. customevaporated
  9. customThe dried material was recrystallized from EtOAc