反应详情

温度

20 °C

To a solution of 2,2-dioxo-6-(1,1-dimethylethyl)-8-iodo-1,2,3-benzoxathiazine (2 g., 5.5 millimole) in methanol (75 ml.) is added sodium borohydride (0.21 g., 5.5 millimole) portionwise with stirring at 20° C. The resulting reaction solution is stirred at 20° C. for 16 hours and then concentrated in vacuo leaving a residual solid which is triturated with water (50 ml.). The insoluble solid is collected and crystallized from 40% ethanol-acetic acid (25:2; v:v) to give 2,2-dioxo-3,4-dihydro-6-(1,1-dimethylethyl)-8-iodo-1,2,3-benzoxathiazine as colorless crystals (1.7 g., 85%), m.p. 154°-155° C.

1. customThe resulting reaction solution
2. stirringis stirred at 20° C. for 16 hours
3. concentrationconcentrated in vacuo
4. customleaving a residual solid which
5. customis triturated with water (50 ml.)
6. customThe insoluble solid is collected
7. customcrystallized from 40% ethanol-acetic acid (25:2; v:v)