反应详情

To a solution of methyl 4-chloro-2-methyl-5-nitrobenzoate (1.21 g) in methanol (20 ml) was added sodium hydrosulfide (561 mg), and the mixture was refluxed with stirring for 2 hours. After the reaction was complete, the reaction solution was concentrated, and methanol was concentrated under reduced pressure. Then, to the resultant were added water and 2N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered, concentrated under reduced pressure. The obtained residue was purified by column chromatography to give the title compound (1.17 g).

1. temperaturethe mixture was refluxed
2. concentrationthe reaction solution was concentrated
3. concentrationmethanol was concentrated under reduced pressure
4. additionThen, to the resultant were added water and 2N hydrochloric acid
5. extractionthe mixture was extracted with ethyl acetate
6. dry with materialThe organic layer was dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe obtained residue was purified by column chromatography