反应详情

In 420 ml of chloroform, 42.0 g (0.14 mole) of the 1′-tert-butoxycarbonyl-spiro[benzo[c]thiophene-1(3H),4′-piperidine] obtained in Referential Example 1(a) were dissolved, followed by the addition of 12.7 g (0.15 mole) of sodium bicarbonate. To the resulting mixture, 28.0 g (85% content, 0.14 mole) of m-chloroperbenzoic acid were added in small portions under ice-cooling. After stirring of the mixture for 30 minutes under ice-cooling, 10 g of potassium iodide were added thereto and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with water and a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure to obtain a residue. The residue was purified by chromatography on a silica gel column (eluting solvent; n-hexane: ethyl acetate=1:1), whereby 42 g of the title compound were obtained as white crystals.

1. dissolutionwere dissolved
2. temperaturecooling
3. temperaturecooling
4. stirringthe mixture was stirred at room temperature for 30 minutes
5. washThe reaction mixture was washed with water
6. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate
7. customthe solvent was removed by distillation under reduced pressure
8. customto obtain a residue
9. customThe residue was purified by chromatography on a silica gel column (eluting solvent; n-hexane: ethyl acetate=1:1)