反应详情

A solution of 2.831 g (8 mmole) 3-iodomethyl-4-iodobutyric acid 17 in 80 mL ethanol is saturated with HCl gas at 0° C. After stirring the solution at room temperature for two days, the solvent is removed under vacuum and the residue is dissolved in dichloromethane. The dichloromethane layer is washed with 10% aqueous sodium bicarbonate (3×100 mL), water (1×100 mL) and brine. The separated dichloromethane layer is dried over with magnesium sulfate, filtered and evaporated to give ethyl-3-iodomethyl-4-iodobutyrate 18.

1. customthe solvent is removed under vacuum
2. dissolutionthe residue is dissolved in dichloromethane
3. washThe dichloromethane layer is washed with 10% aqueous sodium bicarbonate (3×100 mL), water (1×100 mL) and brine
4. dry with materialThe separated dichloromethane layer is dried over with magnesium sulfate
5. filtrationfiltered
6. customevaporated