反应详情

The mixture of 4-chloro-3-methylsulfonyl-5-nitrobenzoic acid (10.0 g) and conc. sulfuric acid (5.0 ml) in methanol (100.0 ml) was heated under reflux for 10 hours and the mixture was evaporated in vacuo. To the residue was added water and the mixture was adjusted to pH 8 with potassium carbonate. The mixture was extracted with a mixture of ethyl acetate and tetrahydrofuran. The extract was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was triturated with diisopropyl ether to give methyl 4-chloro-3-methylsulfonyl-5-nitrobenzoate (10.23 g).

1. temperaturewas heated
2. temperatureunder reflux for 10 hours
3. customthe mixture was evaporated in vacuo
4. additionTo the residue was added water
5. extractionThe mixture was extracted with a mixture of ethyl acetate and tetrahydrofuran
6. washThe extract was washed with brine
7. dry with materialdried over magnesium sulfate
8. customevaporated in vacuo
9. customThe residue was triturated with diisopropyl ether