反应详情

At reflux temperature, a solution of 5.00 g (0.018 mol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate was added dropwise to a solution of 9.60 g (0.072 mol) of lithium iodide and 70 ml of dry pyridine. After stirring under reflux for 2 hours, the reaction mixture was cooled and the solvent was removed under reduced pressure. The residue was then 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 until neutral, dried and concentrated. 4.00 g of 2-chloro-3-formyl-4-methylsulfonylbenzoic acid (85% yield) were obtained.

1. temperatureAt reflux temperature
2. temperatureunder reflux for 2 hours
3. temperaturethe reaction mixture was cooled
4. customthe solvent was removed under reduced pressure
5. extractionThe aqueous phase was extracted with ethyl acetate
6. washthe combined organic phases were washed with water until neutral,
7. customdried
8. concentrationconcentrated