反应详情

6-(Allyloxy)-1,3-benzoxathiol-2-one (48.3 g, 0.232 mol) was dissolved in aq. NaOH solution (2M, 300 ml) and THF (300 ml) to give a yellow solution which stirred at RT for 2 h. The THF was removed in vacuo, a small amount of precipitated starting material removed by filtration, and further starting material was removed by extraction of the aqueous phase into diethyl ether (3×300 ml). The aqueous phase was then acidified to pH 1 with cHCl (˜150 ml) with ice-cooling. Gas evolution was observed, and after 15 min, the title compound was obtained following extraction into diethyl ether (3×300 ml), drying over MgSO4 and concentration to a yellow oil (37.84 g, 0.18 mol).

1. customThe THF was removed in vacuo
2. customa small amount of precipitated
3. customremoved by filtration
4. customwas removed by extraction of the aqueous phase into diethyl ether (3×300 ml)
5. temperaturecooling
6. waitafter 15 min