反应详情

By the method of Yakugaku Zasshi, 87, 387 (1967), 2,6-dimethyl-3-nitro-4-pyridone (11.23 g, 66.8 mmol) and phosphorus oxychloride (57 ml) were heated together at reflux for 1 1/2 hours. The excess reagent was removed under reduced pressure, and the residue dissolved in dichloromethane (150 ml). This solution was treated with dilute aqueous sodium bicarbonate until the aqueous layer was at p87, and then the organic phase was separated, dried (MgSO4) and concentrated under reduced pressure to give a pale yellow solid, (9.8 g, 79%). Caution: this compound is believed to be a powerful skin irritant. 1H NMR (300 MHz, CDCl3) 2.58 (3H, s), 2.61 (3H, s), 7.22 (1H, s).

1. temperatureat reflux for 1 1/2 hours
2. customThe excess reagent was removed under reduced pressure
3. dissolutionthe residue dissolved in dichloromethane (150 ml)
4. additionThis solution was treated with dilute aqueous sodium bicarbonate until the aqueous layer
5. customthe organic phase was separated
6. dry with materialdried (MgSO4)
7. concentrationconcentrated under reduced pressure
8. customto give a pale yellow solid, (9.8 g, 79%)