反应详情

Methanesulfonic acid 3-[4-((R)-2,2-dimethyl[1,3]dioxolan-4-ylmethoxy)-phenyl]-propylester (11.8 g, 34.2 mmol) in acetone (200 mL) is treated with lithium bromide (8.9 g, 100 mmol) and then heated to reflux for 5 h. After cooling to RT the mixture is concentrated in vacuo. The resulting residue is dissolved in EtOAc (150 mL), washed with water (2×50 mL), brine then dried (MgSO4), filtered and concentrated in vacuo to give an oil. Purification by flash chromatography (SiO2, iso-hexane:EtOAc, 4:1) gives the title compound as colourless oil that solidifies upon standing.

1. temperatureheated
2. temperatureto reflux for 5 h
3. concentrationis concentrated in vacuo
4. dissolutionThe resulting residue is dissolved in EtOAc (150 mL)
5. washwashed with water (2×50 mL), brine
6. dry with materialthen dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customto give an oil
10. customPurification by flash chromatography (SiO2, iso-hexane:EtOAc, 4:1)