反应详情

To 45 mL of diethylene glycol was added 5.04 g (90 mmol) of KOH, and the mixture was stirred until solution was complete. To this was added 5.05 g (30 mmol) of 2.2-dimethyl-1-thiophenyl-1-propanone (Lancaster Chemical Co.), and 3.75 g of hydrazine monohydrate, and the reaction was stirred at reflux for 48 hours. The solution was cooled, diluted with 100 mL of 1N HCl and 100 mL of water, and extracted with pentane. The extract was dried over MgSO4, filtered and concentrated to give 4.31 g of the title product. NMR (CDCl3) δ:0.95 (s, 9H), 2.70 (s, 2H), 6.75 (dd, 1H, J=1, J=4 Hz), 6.98 (dd, 1H, J=4, J=6 Hz), 7.12 (dd, 1H, J=1, J=6 Hz).

1. stirringthe reaction was stirred
2. temperatureat reflux for 48 hours
3. temperatureThe solution was cooled
4. extractionextracted with pentane
5. dry with materialThe extract was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated