反应详情

A mixture of EXAMPLE 307C (1.6 g) and 5% HCl (20 mL) in tetrahydrofuran (20 mL) was heated at 80° C. overnight. The solvent was removed to dryness. This solid was re-dissolved and added to tetrahydrofuran (50 mL). To this mixture were added BOC2O (di-t-butyl-dicarbonate) (1.118 g), triethylamine (0.72 mL), and 4-dimethylamionpyridine (1.4 g). The solvent was removed, and the residue was partitioned between water and ethyl acetate. The reaction mixture was stirred overnight. The organic layers were dried (MgSO4), filtered, and concentrated. The residue was purified by Prep HPLC eluting with 20-100% acetonitrile/water with 0.1% trifluoroacetic acid to give the title compound.

1. customThe solvent was removed to dryness
2. dissolutionThis solid was re-dissolved
3. additionadded to tetrahydrofuran (50 mL)
4. additionTo this mixture were added BOC2O (di-t-butyl-dicarbonate) (1.118 g), triethylamine (0.72 mL), and 4-dimethylamionpyridine (1.4 g)
5. customThe solvent was removed
6. customthe residue was partitioned between water and ethyl acetate
7. dry with materialThe organic layers were dried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was purified by Prep HPLC
11. washeluting with 20-100% acetonitrile/water with 0.1% trifluoroacetic acid