反应详情

温度

160 °C

A mixture of methyl 3-hydroxy-5-[(1S)-2-hydroxy-1-methylethoxy]benzoate (2.35 g, 10.39 mmol), 5-(azetidin-1-ylcarbonyl)-2,3-dichloropyridine (2.41 g, 10.39 mmol) and potassium carbonate (2.87 g, 20.8 mmol) in acetonitrile (20 mL) was stirred in a microwave reactor at 160° C. for 6 hours. The solvent was removed in vacuo and the residue partitioned between ethyl acetate (50 mL) and water (50 mL). The organic layer was washed with brine (50 mL), dried (MgSO4), and the solvent removed in vacuo. The crude oil was chromatographed on silica, eluting with 30-100% ethyl acetate in isohexane, to give the desired compound as a yellow oil (5.3 g).

1. customThe solvent was removed in vacuo
2. customthe residue partitioned between ethyl acetate (50 mL) and water (50 mL)
3. washThe organic layer was washed with brine (50 mL)
4. dry with materialdried (MgSO4)
5. customthe solvent removed in vacuo
6. customThe crude oil was chromatographed on silica
7. washeluting with 30-100% ethyl acetate in isohexane