反应详情

To a solution of compound A (46.2 mmol) in EtOAc (175 mL) at room temperature was added piperidine (4.57 mL, 46.2 mmol) and the reaction mixture was stirred for 18 h at room temperature. Next the solvent was removed in vacuo and the resulting residue dissolved in minimum amount of EtOAc (˜50 mL) and hexane (˜1 L) was added. The precipitated crude product was filtered off and recrystallised again with EtOAc (˜30 mL) and hexane (˜750 mL). The precipitate was filtered off, washed with hexane and dried in vacuo to afford compound B (28.0 g, 46.2 mmol). LC-MS [M+H] 595.4 (C28H46N6O6S+H, calc: 595.3). Compound B was used without further purification.

1. customNext the solvent was removed in vacuo
2. dissolutionthe resulting residue dissolved in minimum amount of EtOAc (˜50 mL) and hexane (˜1 L)
3. additionwas added
4. customThe precipitated crude product
5. filtrationwas filtered off
6. customrecrystallised again with EtOAc (˜30 mL) and hexane (˜750 mL)
7. filtrationThe precipitate was filtered off
8. washwashed with hexane
9. customdried in vacuo