反应详情

A 6 N aqueous NaOH solution (54.8 μL, 323 μmol) was added to a solution of 4-carbamoyl-4-(2-fluoro-4-trifluoromethyl-benzoylamino)-piperidine-1-carboxylic acid tert-butyl ester (100 mg, 231 μmol) in DMSO (0.3 mL), and the mixture was stirred at room temperature for 27 hours. The reaction mixture was quenched with a saturated aqueous ammonium chloride solution and then diluted with EtOAc, and the organic layer was sequentially washed with H2O and saturated brine. The organic layer was dried over MgSO4 and then concentrated under reduced pressure. The resulting residue was purified by column chromatography (CH2Cl2/MeOH=95:5) to give 2-(2-fluoro-4-trifluoromethyl-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-carboxylic acid tert-butyl ester as a white solid (54.5 mg, 57%).

1. customThe reaction mixture was quenched with a saturated aqueous ammonium chloride solution
2. additiondiluted with EtOAc
3. washthe organic layer was sequentially washed with H2O and saturated brine
4. dry with materialThe organic layer was dried over MgSO4
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by column chromatography (CH2Cl2/MeOH=95:5)