反应详情

Compound 16 (2.65 g, 15.1 mmol) was dissolved in POCl3 (4.2 ml, 45.3 mmol) under nitrogen atmosphere and refluxed for 2 h. It was then cooled and concentrated under vacuum. The solid concentrate was taken in a beaker with 200 ml water neutralized with NaHCO3 powder and extracted with EtOAc. The solution was dried over Na2SO4, filtered, and concentrated. This crude product was then purified through column chromatography using ethyl acetate to get 17 as brown solid (2.113 g, 72%). 1H NMR (400 MHz, CDCl3) δ ppm 4.079 (s, 3H), 7.08-7.1 (d, 1H, J=8 Hz), 7.49-7.56 (m, 2H), 7.76-7.78 (d, 1H, J=8 Hz), 8.76-8.77 (d, 1H, J=4 Hz).

1. temperaturerefluxed for 2 h
2. temperatureIt was then cooled
3. concentrationconcentrated under vacuum
4. concentrationThe solid concentrate
5. extractionextracted with EtOAc
6. dry with materialThe solution was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThis crude product was then purified through column chromatography