反应详情

温度

140 °C

5,6-Dimethyl-3-nitro-2-pyridone (1-013-04)(841 mg) and phosphorus pentachloride (1.25 g) was heated with stirring in an oil bath at 140° C. under nitrogen atmosphere. After 35 min, the reaction mixture was cooled under ice-cooling, poured into ice-water, extracted with twice with chloroform, and washed once with water and a saturated aqueous solution of sodium bicarbonate. To the extract was added a decolorzing charcoal, and the extract was dried over magnesium sulfate, and evaporated under reduced pressure to give 2-chloro-5,6-dimethyl-3-nitropyridine (1-013-05) (842 mg, 90.2%) as a crystalline residue.

1. temperaturethe reaction mixture was cooled under ice-
2. temperaturecooling
3. extractionextracted with twice with chloroform
4. washwashed once with water
5. additionTo the extract was added a decolorzing charcoal
6. dry with materialthe extract was dried over magnesium sulfate
7. customevaporated under reduced pressure