HRID23527

反应详情

EQUATION

反应方程式

HRID 23527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 3,4-dichlorobenzoic acid (1.0 g, 5.24 mmol) in CH2Cl2 (25 mL) was added N,O-dimethylhydroxylamine hydrochloride (613 mg, 6.28 mmol) followed by N-methylmorpholine (865 μL, 7.85 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.2 g, 6.28 mmol) at which point the reaction mixture became homogeneous. After 2 h, the reaction mixture was diluted with EtOAc and washed with 1N HCl, H2O, saturated NaHCO3 solution and brine, sequentially. The organic layer was dried over Na2SO4, and the removal of solvent in vacuo gave the title compound (1.16 g) that required no further purification.

WORKUP

后处理

  1. washwashed with 1N HCl, H2O, saturated NaHCO3 solution and brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customthe removal of solvent in vacuo