反应详情

A methanol (40 mml) solution of 5-chloro-2-nitropyridine (2.0 g, 12.6 mmol) was added dropwise to a methanol (20 ml) solution of sodium thiomethoxide (1.02 g, 13.9 mmol) while being cooled with ice, and after the mixture was stirred for 13 hours while raising its temperature to the room temperature, water added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water and then with a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. Thereafter, the solvent was distilled off, and the resulting crude product was recrystalized with ethyl acetate-hexane to obtain 972 mg (yield 45%) of 5-methylthio-2-nitropyridine.

1. temperaturewhile being cooled with ice
2. additionadded to the reaction mixture
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with water
5. dry with materialwith a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
6. distillationThereafter, the solvent was distilled off
7. customthe resulting crude product was recrystalized with ethyl acetate-hexane