反应详情

45.9 gm (0.169 mol) of 4-(2'-fluoro-4-biphenylyl)-4-oxo-butyric acid were dissolved in a solution of 11.2 gm of potassium hydroxide in 450 ml of water at 35° C. While stirring, a solution of 6.4 gm (0.169 mol) of sodium borohydride in water was added. After stirring for about 3 hours, the mixture was acidified and extracted with ethyl acetate. From the washed and dried organic phase, the cyclohexylamine salt was precipitated by addition of cyclohexylamine. Yield: 41 gm (65% of theory); m.p. 174°-175° C.; melting point of the free acid: 120°-122° C. (from benzene); melting point of the isobutylamine salt: 125°-127° C. (from isopropanol); melting point of the morpholine salt: 108°-110° C. (from isopropanol); melting point of the sodium salt: 222°-224° C. (from ethanol).

1. stirringAfter stirring for about 3 hours
2. extractionextracted with ethyl acetate
3. washFrom the washed
4. customdried organic phase, the cyclohexylamine salt was precipitated by addition of cyclohexylamine
5. custom120°-122° C. (from benzene)
6. custom125°-127° C. (from isopropanol)
7. custom108°-110° C. (from isopropanol)
8. custom222°-224° C. (from ethanol)