反应详情

Thionyl chloride (0.1 ml) was added at room temperature to a mixture of compound 1 (0.0002 mol) in EtOH (2 ml). The mixture was stirred at room temperature for 2 hours. Water was added. The mixture was taken up in DCM. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated. The residue (0.15 g) was purified by column chromatography over kromasil® (10 μm) (eluent: DCM/MeOH 98/2). The pure fractions were collected and the solvent was evaporated. The residue (0.03 g) was taken up in DCM and evaporated till dryness, yielding 0.023 g (17%) of compound 10.

1. customThe organic layer was separated
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. customthe solvent was evaporated
5. customThe residue (0.15 g) was purified by column chromatography over kromasil® (10 μm) (eluent: DCM/MeOH 98/2)
6. customThe pure fractions were collected
7. customthe solvent was evaporated
8. customevaporated till dryness