反应详情

温度

80 °C

Potassium tert-butoxide (302 mg, 2.69 mmol) was added to a solution of the resulting 1-(2-{4-[(2-allyloxy-ethyl)-methyl-carbamoyl]-2-methyl-phenyl}-ethanesulfonyl)-4-(3-but-3-enyloxy-4-trifluoromethyl-benzoylamino)-piperidine-4-carboxylic amide in ethanol (6 ml), and the mixture was stirred at 80° C. for 30 minutes. A saturated aqueous ammonium chloride solution, water and saturated brine were sequentially added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to give N-(2-allyloxy-ethyl)-4-{2-[2-(3-but-3-enyloxy-4-trifluoromethyl-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-3,N-dimethyl-benzamide (176 mg).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography