(E)-3-(二甲氨基)-1-(1H-吡咯-2-基)丙-2-烯-1-one

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 39.6 g of 2-acetylpyrrole and 104 ml (87.7 g) of tert-butoxy bis(dimethylamino)methane was heated on a steam bath for 20 minutes. The reaction was allowed to subside, then heating was continued for 6 hours. The mixture solidified then was slurried in hexane with chilling. The crude product was collected, washed with hexane and dried. The solid was dissolved in chloroform containing 5% methanol and filtered through magnesium silicate. The eluent was evaporated in vacuo and the residue was recrystallized from dichloromethane/hexane containing a small amount of methanol. The solid was collected, washed with hexane then dried in vacuo giving 25.1 g of the desired compound as yellow crystals, mp 192°-193° C. (dec.). was heated on a steam bath for 20 minutes heating with chilling The crude product was collected washed with hexane dried The solid was dissolved in chloroform containing 5% methanol filtered through magnesium silicate The eluent was evaporated in vacuo the residue was recrystallized from dichloromethane/hexane containing a small amount of methanol The solid was collected washed with hexane then dried in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 39.6 g of 2-acetylpyrrole and 104 ml (87.7 g) of tert-butoxy bis(dimethylamino)methane was heated on a steam bath for 20 minutes. The reaction was allowed to subside, then heating was continued for 6 hours. The mixture solidified then was slurried in hexane with chilling. The crude product was collected, washed with hexane and dried. The solid was dissolved in chloroform containing 5% methanol and filtered through magnesium silicate. The eluent was evaporated in vacuo and the residue was recrystallized from dichloromethane/hexane containing a small amount of methanol. The solid was collected, washed with hexane then dried in vacuo giving 25.1 g of the desired compound as yellow crystals, mp 192°-193° C. (dec.). was heated on a steam bath for 20 minutes heating with chilling The crude product was collected washed with hexane dried The solid was dissolved in chloroform containing 5% methanol filtered through magnesium silicate The eluent was evaporated in vacuo the residue was recrystallized from dichloromethane/hexane containing a small amount of methanol The solid was collected washed with hexane then dried in vacuo