HRID387823
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
2-Amino-4-(4-amino-3-chlorophenoxy)pyridine (1.0 g), N-bromosuccinimide (0.78 g) and isopropanol (10 ml) were stirred for 15 minutes under reflux. The mixture was returned to room temperature, water was added, and extraction was performed with ethyl acetate. Silica gel was added to the extract solution and the solvent was distilled off under reduced pressure. The silica gel was charged into a dry column packed with silica gel, and purification was performed by column chromatography (hexane:ethyl acetate=2:1, followed by 1:1, ethyl acetate) to obtain 400 mg of the target substance as a brown oil.
WORKUP
后处理
- temperatureunder reflux
- customwas returned to room temperature
- extractionextraction
- additionSilica gel was added to the extract solution
- distillationthe solvent was distilled off under reduced pressure
- additionThe silica gel was charged into a dry column
- custompacked with silica gel, and purification
- customto obtain 400 mg of the target substance as a brown oil