反应详情

A mixture of tert-butyl 4-((2-((2S)-bicyclo[2.2.1]heptan-2-ylamino)-5-methyl-4-oxo-4,5-dihydrothiazol-5-yl)methyl)piperidine-1-carboxylate (1.42 g, 3.37 mmol, 1.0 eq) in 50 mL of a 4.7 M HCl solution in EtOAc was stirred at room temperature. After 4 h, the reaction mixture was concentrated in vacuo. Aqueous Na2CO3 (2.0 M, 20 mL) was then added, and water was removed in vacuo. The residue was then triturated with 10% MeOH—CH2Cl2 (6×100 mL), and the combined triturating solution were concentrated in vacuo. The crude product was dissolved in CH2Cl2, filtered, and concentrated in vacuo to afford the title compound as a light orange solid (1.08 g). MS (ESI, pos. ion) m/z: 322 (M+H).

1. concentrationthe reaction mixture was concentrated in vacuo
2. additionAqueous Na2CO3 (2.0 M, 20 mL) was then added
3. customwater was removed in vacuo
4. customThe residue was then triturated with 10% MeOH—CH2Cl2 (6×100 mL)
5. customthe combined triturating solution
6. concentrationwere concentrated in vacuo
7. dissolutionThe crude product was dissolved in CH2Cl2
8. filtrationfiltered
9. concentrationconcentrated in vacuo