反应详情

温度

236.5 °C

5-{[(5-Bromopyridin-3-yl)imino]methyl}-2,2-dimethyl-1,3-dioxane-4,6-dione (59 g, 0.18 mol) was slowly added to DOWTHERM A heat transfer fluid (2000 mL) over a period of 5 minutes at 235-238° C. Following addition, the reaction was maintained for an additional 5 minutes and then allowed to cool to 40° C. A brown precipitate formed, which was filtered and washed with hexanes (150 mL). The brown solid was suspended in an ethanol/water mixture (90:10, 1500 mL), heated to a boil for 30 minutes, isolated by filtration, and washed with ethanol (200 mL) to yield 30.8 g of 7-bromo[1,5]naphthyridin-4-ol as a dark brown powder.

1. additionaddition
2. temperaturethe reaction was maintained for an additional 5 minutes
3. temperatureto cool to 40° C
4. customA brown precipitate formed
5. filtrationwhich was filtered
6. washwashed with hexanes (150 mL)
7. temperatureheated to a boil for 30 minutes
8. customisolated by filtration
9. washwashed with ethanol (200 mL)