反应详情

Phosphorus oxychloride (25 ml, 0.27 mol) was added to 4-hydroxy-3-nitropyridine (7.0 g, 50.0 mmol), followed by reaction at 80° to 90° C. for 1.5 hours. Phosphorus oxychloride was removed by distillation. About 100 g of ice was added to the residue, and 28% aqueous ammonia was added dropwise thereto to adjust the pH to 7. Then, 100 ml of water was added thereto, and the aqueous mixture was extracted three times with 200 ml of dichloromethane. The resulting dichloromethane layer was dried, and then dichloromethane was removed by distillation under reduced pressure to obtain 7.75 g of a yellow liquid (yield: 97.8%).

1. customfollowed by reaction at 80° to 90° C. for 1.5 hours
2. customPhosphorus oxychloride was removed by distillation
3. additionAbout 100 g of ice was added to the residue, and 28% aqueous ammonia
4. additionwas added dropwise
5. additionThen, 100 ml of water was added
6. extractionthe aqueous mixture was extracted three times with 200 ml of dichloromethane
7. dry with materialThe resulting dichloromethane layer was dried
8. customdichloromethane was removed by distillation under reduced pressure