HRID487200

反应详情

EQUATION

反应方程式

HRID 487200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,5-dichloro-3-nitrobenzoic acid (23.6 g, 100 mmol), powdered potassium carbonate (41.1 g, 300 mmol), and 4-(aminoethyl)benzoic acid (60.04 g, 400 mmol) in 250 ml of methanol was refluxed under argon for 18 hours. The reaction mixture was poured into 650 ml of 10% aqueous hydrochloric acid solution. The solid was collected and triturated with ethyl acetate. The ethyl acetate extract was decanted, dried with magnesium sulfate and concentrated in vacuo to give 20.15 g (57.5%) of the title compound; mp 255°-257° C.

WORKUP

后处理

  1. temperaturewas refluxed under argon for 18 hours
  2. customThe solid was collected
  3. customtriturated with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. customwas decanted
  6. dry with materialdried with magnesium sulfate
  7. concentrationconcentrated in vacuo