反应详情

温度

100 °C

The product of Step C, 1-C, (23.34 g, 82 mmol) was suspended in H2O (66 mL) and cone. HCl (58.1 mL, 708 mmol). The reaction mixture was heated at 100° C. for 24 h. The reaction mixture was cooled to rt and partitioned with MTBE. The organic layer was discarded. The aqueous layer was treated with aq. 5.0 M NaOH (160 mL, 800 mmol) and extracted with EtOAc (2ט700 mL). The combined organic layers were dried (MgSO4), filtered and concentrated under reduced pressure to about ¼ of the original volume. Benzenesulfonic acid (12.98 g, 82 mmol) was added as a solid and the mixture was agitated and allowed to stand at rt for 10 min. The solids were isolated by vacuum filtration, rinsed with hexanes and dried under high vacuum. HPLC/MS: 243.0 (M+1); Rt=1.49 min.

1. temperatureThe reaction mixture was cooled to rt
2. custompartitioned with MTBE
3. extractionextracted with EtOAc (2ט700 mL)
4. dry with materialThe combined organic layers were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure to about ¼ of the original volume
7. customThe solids were isolated by vacuum filtration
8. washrinsed with hexanes
9. customdried under high vacuum