反应详情

Ethyl 4-formyl-5-methyl-1H-pyrrole-2-carboxylate (Intermediate 15, 0.2 g, 1.1 mmol) and hydroxylamine hydrochloride (0.08 g, 1.1 mmol) were dissolved in EtOH (10 ml) and refluxed for 1.5 hours. The mixture was concentrated under vacuum to give yellow solid, which was dissolved in DMF (5 ml) before addition of SOCl2 (0.35 ml) at 0° C. The solvent was removed under vacuum after the completion of the reaction and the residue was partitioned between water and EtOAc. The layers were separated and the aqueous layer was extracted with EtOAc twice. The combined organic extracts were dried over MgSO4 and concentrated to give brown solid (0.16 g, crude).

1. temperaturerefluxed for 1.5 hours
2. concentrationThe mixture was concentrated under vacuum
3. customto give yellow solid, which
4. customThe solvent was removed under vacuum
5. customafter the completion of the reaction
6. customthe residue was partitioned between water and EtOAc
7. customThe layers were separated
8. extractionthe aqueous layer was extracted with EtOAc twice
9. dry with materialThe combined organic extracts were dried over MgSO4
10. concentrationconcentrated
11. customto give brown solid (0.16 g, crude)