反应详情

The product prepared in Step A above (3.55 g, 9 mmol), NH4OAc (ammonium acetate) (20.8 g, 270 mmol) and AcOH (acetic acid) (30 mL) were combined at room temperature and the reaction mixture was warmed on a steam bath for about 3 hours. The reaction mixture was then cooled to room temperature and poured into an ice slurry mix (400 g). To this mixture was added concentrated ammonium hydroxide (50 mL) and ethyl ether. The layers were separated, and the aqueous phase washed with a second portion of ethyl ether. The organic phases were combined, dried over MgSO4, filtered, and concentrated under reduced pressure to yield a brown foam. This sample was purified by preparative HPLC to yield the purified title compound as a white powder. LC indicated the sample was 96% pure at 214 nm.

1. customwere combined at room temperature
2. temperaturethe reaction mixture was warmed on a steam bath for about 3 hours
3. additionmix (400 g)
4. customThe layers were separated
5. washthe aqueous phase washed with a second portion of ethyl ether
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customto yield a brown foam
10. customThis sample was purified by preparative HPLC
11. customto yield the
12. custompurified title compound as a white powder