反应详情

To a solution of 1.3 g 5-[2-((S)-2-carboxy-pyrrolidin-1-yl)-2-oxo-ethoxy]-1-phenyl-1H-pyrazole-3-carboxylic acid ethyl ester in 20 ml DMF were added 1.28 g HATU and 0.56 ml DIPEA. After 10 minutes 334 mg 2-fluoroethylamine hydrochloride were added. Additional 100 mg 2-fluoroethylamine hydrochloride and 400 mg HATU were added after 2 h. The reaction mixture was allowed to stir for further 12 h before being diluted with dichloromethane and extracted with aqueous LiCl (4%), 0.1 M HCl and saturated NaHCO3. The crude product obtained after evaporation of the solvent was purified by flash chromatography on silica using ethyl acetate/heptane 80:20 to ethyl acetate/heptane 100:0 as eluent. Yield: 1.5 g colorless oil.

1. extractionextracted with aqueous LiCl (4%), 0.1 M HCl and saturated NaHCO3