反应详情

A solution of 3-[(2-hydroxyethoxy)methyl]benzonitrile (1 g) in MeOH (20 ml) was treated with conc. H2SO4 (10 ml) at 0° C. The solution was then allowed to warm to room temperature before heating at reflux for 10 h. Aqueous sodium carbonate was added to neutralise the cooled solution before extracting with EtOAc. The combined organic layers were then washed with water, dried (MgSO4) and concentrated in vacuo. The residue was then purified by chromatography (Biotage, 90 g) eluting with 40°C.-60° C. petroleum ether-EtOAc (3:2) to give the title compound (650 mg). LCMS RT=2.33 min.

1. temperaturebefore heating
2. temperatureat reflux for 10 h
3. extractionbefore extracting with EtOAc
4. washThe combined organic layers were then washed with water
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe residue was then purified by chromatography (Biotage, 90 g)
8. washeluting with 40°C.-60° C. petroleum ether-EtOAc (3:2)