反应详情

温度

-3 °C

2.65 g (10 mmoles) of 2-[3-chloro-4-(4-aminopyrazol-1-yl)phenyl]propionic acid are dissolved in 10 ml of 25% strength hydrochloric acid, the solution is cooled to -3° C., and 1.04 g (15 mmoles) of sodium nitrite (dissolved in 5 ml of water) are added. After 10 minutes the reaction mixture is stirred into a solution of 2 g (20 mmoles) of copper(I) chloride. Heating to 100° C. ist then effected for 1 hour, followed by cooling, extraction with chloroform and purification through chromatography on silica gel (benzene/cyclohexane/glacial acetic acid 2:1:1). 2-[3-chloro-4-(4-chloropyrazol-1-yl)phenyl]propionic acid, m.p. 102°-103° C., is obtained.

1. temperatureHeating to 100° C.
2. temperatureby cooling
3. extractionextraction
4. customwith chloroform and purification through chromatography on silica gel (benzene/cyclohexane/glacial acetic acid 2:1:1)