反应详情

An amount of 3.415 g (9 mmol) of the product of Step B was dissolved in 19 mL of methanol. It was cooled in an ice-bath and 1.13 mL of thionyl chloride was added dropwise. The mixture was heated at reflux for 30 min. It was cooled and the methanol removed under reduced pressure. A saturated solution of sodium bicarbonate was carefully added to the residue, then extracted with ether. The combined ether extracts were washed with brine, dried (MgSO4) and concentrated to give a white solid: mp 123°-124° C. 1H-NMR (DMSO-d6) δ9.90 (d, 1H), 7.55 (m, 1H), 7.20 (m,3H), 7.00 (d, 1H), 5.90 (d, 1H), 3.75 (s,3H).

1. temperatureIt was cooled in an ice-bath
2. temperatureThe mixture was heated
3. temperatureat reflux for 30 min
4. temperatureIt was cooled
5. customthe methanol removed under reduced pressure
6. additionA saturated solution of sodium bicarbonate was carefully added to the residue
7. extractionextracted with ether
8. washThe combined ether extracts were washed with brine
9. dry with materialdried (MgSO4)
10. concentrationconcentrated
11. customto give a white solid