HRID382857

反应详情

EQUATION

反应方程式

HRID 382857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.7 g (0.04 mol) of methyl 3-chlorocarbonyl-2,4-dichlorobenzoate in 100 ml of methylene chloride were slowly added dropwise at 30° C. to a solution of 4.50 g (0.04 mol) of propoxyamine hydrochloride and 4.05 g (0.04 mol) of triethylamine in 200 ml of methylene chloride. After the reaction mixture had been stirred for 2 hours at room temperature, it was washed with dilute phosphoric acid, dried and concentrated. The resulting residue was chromatographed on silica gel (eluent: toluene/ethyl acetate=9/1). This gave 11.50 g of methyl 2,4-dichloro-3-(N-propoxyamino)carbonylbenzoate.

WORKUP

后处理

  1. washit was washed with dilute phosphoric acid
  2. customdried
  3. concentrationconcentrated
  4. customThe resulting residue was chromatographed on silica gel (eluent: toluene/ethyl acetate=9/1)