反应详情

A mixture of intermediate (19) (0.079 mol) and MgSO4 (35.5 g) in toluene (500 ml) was stirred and refluxed overnight in a Dean-Stark apparatus and then cooled. The precipitate was filtered off and the filtrate was evaporated till dryness. The residue (35 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/EtOAc 85/15; 20–45 μm). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from acetonitrile and DIPE. The precipitate was filtered off and dried, yielding 1.5 g (4.4%) of 7-(4-chlorobenzoyl)-5-(3-chlorophenyl)-1,5-dihydro-4,1-benzothiazepin-2(3H)-one (intermediate 20), mp. 222° C.

1. temperaturerefluxed overnight in a Dean-Stark apparatus
2. temperaturecooled
3. filtrationThe precipitate was filtered off
4. customthe filtrate was evaporated till dryness
5. customThe residue (35 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/EtOAc 85/15; 20–45 μm)
6. customThe pure fractions were collected
7. customthe solvent was evaporated
8. customThe residue was crystallized from acetonitrile and DIPE
9. filtrationThe precipitate was filtered off
10. customdried