反应详情

温度

70 °C

With reference to the method disclosed in Chemical and Pharmaceutical Bulletin, vol. 16, No. 7, pages 1300 to 1307 (1968), 10 g of 2-hydroxycycloheptimidazole, 150 g of phosphorus oxychloride and 12 g of N,N-diethylaniline were stirred with heating to the inner temperature of 70° C. for 6 hours and 30 minutes. After the reaction, phosphorus oxychloride was distilled away under reduced pressure and 500 ml of ice water was added to the residue. Then, a sodium bicarbonate solution was added thereto to neutral pH, and extracted with chloroform (250 ml×2). The chloroform layer was dried over anhydrous sodium sulfate, solvent was distilled away, and the residue was purified by silica gel column chromatography using ethyl acetate as a developing solvent.

1. distillationwas distilled away under reduced pressure and 500 ml of ice water
2. additionwas added to the residue
3. additionThen, a sodium bicarbonate solution was added
4. extractionto neutral pH, and extracted with chloroform (250 ml×2)
5. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate, solvent
6. distillationwas distilled away
7. customthe residue was purified by silica gel column chromatography