反应详情

温度

22.5 °C

A solution of 0.97 g of 1-(para-chlorophenyl)-3-hydroxypyrazole in 20 ml of anhydrous dimethylformamide (DMF) was admixed with 0.13 g of sodium hydride and then stirred at 20-25 ° C. for approximately one hour. 1.34 g of the oxime from Example 2 were then added and the mixture was stirred at 60° C. for approximately three hours and then at 20-25° C. for approximately 14 hours. 300 ml of water were added and the mixture was then extracted with methyl tert-butyl ether (MTBE). The combined organic phases were washed with water and dried, and the solvent was then removed. The residue was chromatographed over silica gel (cyclohexane/ethyl acetate mixture [1:1]), giving 1.15 g of the title compound as a light-beige amorphous powder of m.p. 56-59° C.

1. stirringthe mixture was stirred at 60° C. for approximately three hours
2. waitat 20-25° C. for approximately 14 hours
3. extractionthe mixture was then extracted with methyl tert-butyl ether (MTBE)
4. washThe combined organic phases were washed with water
5. customdried
6. customthe solvent was then removed
7. customThe residue was chromatographed over silica gel (cyclohexane/ethyl acetate mixture [1:1])