反应详情

温度

2.5 °C

10.0 g of the crude tert-butyl spiro[benzo[c]thiophene-1(3H),4′-piperidine]-1′-carboxylate, obtained in Example 1, were added to 50 ml of methylene chloride and 150 ml of acetone followed by cooling to 0 to 5° C. A solution of 15.0 g (24.4 mmol) of Oxone™ in 75 ml of water was dropped in at 5° C. or lower followed by stirring for 3 hours at 0 to 5° C. A solution of 1.72 g (9.8 mmol) of sodium thiosulfate-hydrate in 50 ml of water was added followed by stirring for 30 minutes at 20 to 25° C. 100 ml of methylene chloride and 100 ml of water were then added followed by separation of the aqueous layer. After washing the organic layer with 100 ml of water, it was dried with anhydrous magnesium sulfate followed by distilling off the solvent to obtain 10.5 g of tert-butyl spiro[benzo[c]thiophene-1-(3H),4′-piperidine]-1′-carboxylate 2-oxide as a white foamy substance (crude yield: 100%).

1. stirringby stirring for 30 minutes at 20 to 25° C
2. customfollowed by separation of the aqueous layer
3. washAfter washing the organic layer with 100 ml of water, it
4. dry with materialwas dried with anhydrous magnesium sulfate
5. distillationby distilling off the solvent