反应详情

Methyl 3-hydroxy-2-nitrobenzoate (95 g, 0.52 mol), tetrahydro-2H-pyran-4-yl methanesulfonate (234 g, 1.3 mol) and K2CO3 (358 g, 2.6 mol) was suspend in MeCN (2 L). The mixture was heated at reflux for 20 h. TLC (petroleum ether:ethyl acetate=1:1) showed the reaction was complete. The mixture was filtered; the filtrate was concentrated in vacuo. The residue was purified by chromatography (petroleum ether: ethyl acetate=10:1, 5:1, 2:1) to give the title compound (200 g 100%) as a yellow oil.

1. temperatureThe mixture was heated
2. temperatureat reflux for 20 h
3. filtrationThe mixture was filtered
4. concentrationthe filtrate was concentrated in vacuo
5. customThe residue was purified by chromatography (petroleum ether: ethyl acetate=10:1, 5:1, 2:1)