反应详情

To a reaction vessel, all compound XV obtained in the above step and 750 ml ethanol were added. The mixture was heated until dissolved completely, 36 ml concentrated hydrochloric acid was added, the reaction was kept at about 50-55° C. for 5 h, concentrated to about 200 ml under reduced pressure, 900 ml ethyl acetate was added dropwise, cooled and filtered, the filter cake was washed and dried, and 24.3 g compound II-5 was obtained, with yield of 46.2% (calculated according to compound IX-1). 1H NMR (D2O): δ 1.06 (t, 2H, J=6.7 Hz), 1.32-1.46 (m, 6H), 1.60 (m, 1H), 1.91 (d, 2H, J=13.5 Hz), 2.91-3.03 (m, 4H), 3.39 (d, 2H, J=12.8 Hz), 5.90 (s, 2H), 6.18 (s, 1H), 6.68 (s, 1H); MS (ESI): m/z 315 [M-Cl]+.

1. additionwere added
2. temperatureThe mixture was heated
3. dissolutionuntil dissolved completely
4. concentrationconcentrated to about 200 ml under reduced pressure, 900 ml ethyl acetate
5. additionwas added dropwise
6. temperaturecooled
7. filtrationfiltered
8. washthe filter cake was washed
9. customdried
10. customwas obtained, with yield of 46.2% (calculated according to compound IX-1)