HRID449895

反应详情

EQUATION

反应方程式

HRID 449895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customat room temperature
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel
  6. washeluting with petroleum-diethyl:ether (50:1)