反应详情

A solution of the crude ether from Example 2 (35.0 g) and 80 ml trifluoroacetic acid was stirred at room temperature for 16 hours. The trifluoroacetic acid was removed in vacuo and methylene chloride added to the residue. The organic phase was washed twice with cold saturated sodium bicarbonate, once with water and dried (Na2SO4). Concentration gave a viscous brown oil which was triturated with hexane. The resulting sticky solid was recrystallized from chloroform/hexane (1:1) to provide 11.0 g of pure 2-(2-methoxyethyl)benzenesulfonamide as a white solid; m.p. 79-81.

1. customThe trifluoroacetic acid was removed in vacuo and methylene chloride
2. additionadded to the residue
3. washThe organic phase was washed twice with cold saturated sodium bicarbonate, once with water
4. dry with materialdried (Na2SO4)
5. concentrationConcentration
6. customgave a viscous brown oil which
7. customwas triturated with hexane
8. customThe resulting sticky solid was recrystallized from chloroform/hexane (1:1)