反应详情

To a solution of 3-bromo-2,2-bis(bromomethyl)propanol (127) (3.25 g, 10 mmol) and potassium hydroxide (1.12 g, 20 mmol, in 10 mL water) in EtOH (20 mL) were added toluene-4-sulfonamide (3.76 g, 22 mmol). The reaction mixture was refluxed for 2 h, evaporated to remove EtOH then diluted with EAOAc (20 mL), washed with H2O (20 mL). The organic layer was washed with brine (20 mL), dried over Na2SO4, and filtered, evaporated to give the product to give 6-(toluene-4-sulfonyl)-2-oxa-6-aza-spiro[3.3]heptane (128) (1.6 g, 6.3 mmol, yield: 63%).

1. temperatureThe reaction mixture was refluxed for 2 h
2. customevaporated
3. customto remove EtOH
4. additionthen diluted with EAOAc (20 mL)
5. washwashed with H2O (20 mL)
6. washThe organic layer was washed with brine (20 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated
10. customto give the product