HRID449895
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
To a solution of dimethyl 2-amino-3,5-dichloroterephthalate (200 g, 0.72 mol) in THF (1 L) at room temperature was slowly added isoamylnitrite (240 mL). The mixture was heated under reflux for 3 hours, cooled to room temperature and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with petroleum-diethyl:ether (50:1) to give dimethyl 2,6-dichloroterephthalate (187 g, yield: 98%) as a light yellow solid.
WORKUP
后处理
- customat room temperature
- temperatureThe mixture was heated
- temperatureunder reflux for 3 hours
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography on silica gel
- washeluting with petroleum-diethyl:ether (50:1)