反应详情

温度

60 °C

Phosphorous oxychloride (63.4 mL, 0.68 mol) was added dropwise to a stirred mixture of 2,4-dihydroxy-3-nitropyridine (28.92 g, 0.17 mol) and benzyl triethylammonium chloride (155 g, 0.68 mol) in acetonitrile (560 mL). The reaction mixture was warmed to 60° C. for 1 h then was heated to reflux for 1 h. The reaction was cooled and the volatiles were evaporated in vacuo. An ice/water slurry (500 mL) was added to the residual oil and the mixture was stirred for 3 h at 0° C. The solids were collected by filtration, washing with water and hexanes to give the title compound as a solid;

1. temperaturethen was heated
2. temperatureto reflux for 1 h
3. temperatureThe reaction was cooled
4. customthe volatiles were evaporated in vacuo
5. additionAn ice/water slurry (500 mL) was added to the residual oil
6. filtrationThe solids were collected by filtration
7. washwashing with water and hexanes