反应详情

A solution of 5.00 g of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate was slowly added dropwise to a solution of 9.60 g (0.072 mol) of lithium iodide and 70 ml of dry pyridine at reflux temperature. After the reaction mixture had been stirred for 2 hours under reflux it was cooled, and the solvent was removed in vacuo. The residue was subsequently taken up in water and brought to pH 1-2 using dilute hydrochloric acid. After the aqueous phase had been extracted with ethyl acetate, the combined organic phases were washed to neutrality with water, dried and concentrated. This gave 4.00 g of 2-chloro-3-formyl-4-methylsulfonylbenzoic acid (85% yield).

1. temperatureat reflux temperature
2. temperatureunder reflux it
3. temperaturewas cooled
4. customthe solvent was removed in vacuo
5. extractionAfter the aqueous phase had been extracted with ethyl acetate
6. washthe combined organic phases were washed
7. customdried
8. concentrationconcentrated