反应详情

温度

70 °C

In accordance with the method described 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 under heating at an internal temperature of 70° C. for 6 hours and 30 minutes. After the reaction, the phosphorus oxychloride was evaporated off under reduced pressure, and the resulting reaction mixture was poured into 500 ml of ice-water. Sodium hydrogencarbonate was added to the resulting solution until the pH thereof became neutral, and this was extracted with chloroform (250 ml×2). The chloroform layer was dried with anhydrous sodium sulfate and the solvent was evaporated off, and then the reaction product was purified by silica gel column chromatography with a developer solvent of ethyl acetate. 2.7 g of colorless crystals were obtained.

1. customAfter the reaction
2. customthe phosphorus oxychloride was evaporated off under reduced pressure
3. customthe resulting reaction mixture
4. extractionthis was extracted with chloroform (250 ml×2)
5. dry with materialThe chloroform layer was dried with anhydrous sodium sulfate
6. customthe solvent was evaporated off
7. customthe reaction product was purified by silica gel column chromatography with a developer solvent of ethyl acetate