反应详情

To a suspension of aluminium chloride (22.9 g, 172 mmol) in anhydrous dichloromethane (100 ml) and acetylchloride (4.5 g, 57.3 mmol)was added a solution of 1-methyl pyrrole-2-carboxaldehyde (5 g, 46 mmol) in anhydrous. dichloromethane (20 ml). The mixture was refluxed for 90 min, poured into ice and stirred until melted. The layers were separated and aqueous layer was extracted with dichloromethane (2×100 ml). The organic phase and extracts were combined, dried over sodium sulfate. The solvent was removed in vacuo to give the title compound (6.8 g, 94%), 1H NMR (d6-DMSO) d 9.6 (s, 1H), 7.9 (s, 1H), 7.4 (s, 1H), 3.9 (s, 3H),2.4 (s,3H)

1. temperatureThe mixture was refluxed for 90 min
2. additionpoured into ice
3. customThe layers were separated
4. extractionaqueous layer was extracted with dichloromethane (2×100 ml)
5. dry with materialdried over sodium sulfate
6. customThe solvent was removed in vacuo