反应详情

A flask was charge with 9.54 g (34.3 mmol) of (2S)-methanesulfonic acid 2-(2,4-difluoro-benzyl)-butyl ester, 10.3 g (68.6 mmol) of sodium iodide, and 60 mL of acetone. The solution was heated at reflux for 30 hours. The acetone was removed under reduced pressure. The residue was partitioned between water and hexanes. The organic layer was collected and washed with sodium bisulfite solution and brine. The hexane was removed under reduced pressure, and the crude oil was purified by column chromatography (hexanes eluent). This procedure gave 9.7 g (91% yield) of the titled compound as a clear oil.

1. temperatureThe solution was heated
2. temperatureat reflux for 30 hours
3. customThe acetone was removed under reduced pressure
4. customThe residue was partitioned between water and hexanes
5. customThe organic layer was collected
6. washwashed with sodium bisulfite solution and brine
7. customThe hexane was removed under reduced pressure
8. customthe crude oil was purified by column chromatography (hexanes eluent)