HRID41330
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
- -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
- customforming a yellow slurry
- additionthe suspension was poured through a frit
- washthe solid washed with water
- dissolutionThe orange solid was dissolved in 300 mL CH2Cl2
- extractionextracted with 3×100 mL water
- dry with materialdried over MgSO4
- filtrationfiltered
- customto give a red solution
- customThe solvent was removed under vacuum
- customto give a red oil