HRID1368816

反应详情

EQUATION

反应方程式

HRID 1368816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.37 g (0.0137 mol) of methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate was slowly added dropwise to 7.29 g (0.055 mol) of lithium iodide in 50 ml of dry pyridine. After stirring for 2 hours at reflux, the reaction mixture was cooled and the solvent was removed under reduced pressure. The residue was taken up in water and adjusted to pH=1-2 with dilute hydrochloric acid. The aqueous phase was extracted with ethyl acetate and the combined organic phases were washed with water, dried and concentrated under reduced pressure. 3.70 g of 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid were obtained. (Yield 89%).

WORKUP

后处理

  1. temperatureat reflux
  2. temperaturethe reaction mixture was cooled
  3. customthe solvent was removed under reduced pressure
  4. extractionThe aqueous phase was extracted with ethyl acetate
  5. washthe combined organic phases were washed with water
  6. customdried
  7. concentrationconcentrated under reduced pressure