反应详情

To a stirred solution of racemic tert-butyl 4-((2R,3S,4R,5S)-3-(3-chloro-2-fluorophenyl)-4-(4-chloro-2-fluorophenyl)-4-cyano-5-neopentylpyrrolidine-2-carboxamido)-4-methylpiperidine-1-carboxylate (27.0 mg, 0.0407 mmol, example 386) in dichloromethane (3 mL) was added TRIFLUOROACETIC ACID (4.44 g, 3 mL) and the reaction mixture was stirred at 0˜5 C for 2.5 hrs. The solvent was removed in vacuum and residue was dissolved in CH2Cl2 (80 mL), washed with sat Na2CO3 (15 mL), water (2×15 mL) and evaporated to give rac-(2R,3S,4R,5S)-4-(4-Chloro-2-fluoro-phenyl)-3-(3-chloro-2-fluoro-phenyl)-4-cyano-5-(2,2-dimethyl-propyl)-pyrrolidine-2-carboxylic acid (4-methyl-piperidin-4-yl)-amide as a white solid. MS (ES+) m/z Calcd: [(M+H)+]: 563. found: 563.

1. customThe solvent was removed in vacuum and residue
2. dissolutionwas dissolved in CH2Cl2 (80 mL)
3. washwashed with sat Na2CO3 (15 mL), water (2×15 mL)
4. customevaporated