HRID349472

反应详情

EQUATION

反应方程式

HRID 349472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-[(4-chloro-N-chloro-benzimidoyl)-amino]-4-methoxy-benzoic acid methyl ester (5.5 g, 15.63 mmol) obtained in step 1 was dissolved in 40 ml of 50% methanol and Na2CO3 (3.53 g, 33.26 mmol) was added dropwise thereto at room temperature and refluxed for 5 min. The resulting solution was cooled to room temperature, extracted with ethyl acetate, the extract was concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (2.57 g, 8.13 mmol) in a yield of 52%.

WORKUP

后处理

  1. temperatureThe resulting solution was cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. concentrationthe extract was concentrated under a reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography