HRID41330

反应详情

EQUATION

反应方程式

HRID 41330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-35 °C

PROCEDURE

实验过程

To a slurry of 2-amino-4-methylphenol (4.40 g, 35.7 mmol) in 300 mL water, a water solution of pyridine-2-carbaldehyde (3.80 g, 35.5 mmol) was slowly added, forming a yellow slurry. After stirring overnight, the suspension was poured through a frit and the solid washed with water. The orange solid was dissolved in 300 mL CH2Cl2 and extracted with 3×100 mL water, dried over MgSO4 and filtered to give a red solution. The solvent was removed under vacuum to give a red oil. The oil was re-dissolved in CH2Cl2, layered with an equal volume of hexane and cooled to −35° C. to yield yellow crystals of 11(5.56 g, 73% yield).

WORKUP

后处理

  1. customforming a yellow slurry
  2. additionthe suspension was poured through a frit
  3. washthe solid washed with water
  4. dissolutionThe orange solid was dissolved in 300 mL CH2Cl2
  5. extractionextracted with 3×100 mL water
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customto give a red solution
  9. customThe solvent was removed under vacuum
  10. customto give a red oil