2-甲氧基-N,N-二甲基乙酰胺

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 14.5 g (61.2 mmol) of 2,6-dibrompyridine were dissolved in about 50 ml of THF, and 35 ml of 2 M isopropylmagnesium chloride (corresponds to 70 mmol) were added under argon. The temperature of the mixture increased. The mixture was stirred at room temperature for another 1.5 h and at 30° C. for 2 h and then cooled in a CO2/EtOH bath, and a solution of 8 g (68.2 mmol) of 2-methoxy-N,N-dimethylacetamide in THF was added, the thickened reaction material was diluted with more THF and allowed to thaw, ethyl acetate, aq. citric acid, dil. aqueous sodium hydroxide solution to pH=6, aq. NaCl were added, the aqueous phase was extracted three times with ethyl acetate and the combined organic phases were dried with MgSO4 and concentrated by evaporation. The residue was distilled under reduced pressure in a kugelrohr and the distillate was recrystallized from a little benzotrifluoride. The temperature of the mixture increased cooled in a CO2/EtOH bath were added the aqueous phase was extracted three times with ethyl acetate the combined organic phases were dried with MgSO4 concentrated by evaporation The residue was distilled under reduced pressure in a kugelrohr the distillate was recrystallized from a little benzotrifluoride

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 14.5 g (61.2 mmol) of 2,6-dibrompyridine were dissolved in about 50 ml of THF, and 35 ml of 2 M isopropylmagnesium chloride (corresponds to 70 mmol) were added under argon. The temperature of the mixture increased. The mixture was stirred at room temperature for another 1.5 h and at 30° C. for 2 h and then cooled in a CO2/EtOH bath, and a solution of 8 g (68.2 mmol) of 2-methoxy-N,N-dimethylacetamide in THF was added, the thickened reaction material was diluted with more THF and allowed to thaw, ethyl acetate, aq. citric acid, dil. aqueous sodium hydroxide solution to pH=6, aq. NaCl were added, the aqueous phase was extracted three times with ethyl acetate and the combined organic phases were dried with MgSO4 and concentrated by evaporation. The residue was distilled under reduced pressure in a kugelrohr and the distillate was recrystallized from a little benzotrifluoride. The temperature of the mixture increased cooled in a CO2/EtOH bath were added the aqueous phase was extracted three times with ethyl acetate the combined organic phases were dried with MgSO4 concentrated by evaporation The residue was distilled under reduced pressure in a kugelrohr the distillate was recrystallized from a little benzotrifluoride

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 14.5 g (61.2 mmol) of 2,6-dibrompyridine were dissolved in about 50 ml of THF, and 35 ml of 2 M isopropylmagnesium chloride (corresponds to 70 mmol) were added under argon. The temperature of the mixture increased. The mixture was stirred at room temperature for another 1.5 h and at 30° C. for 2 h and then cooled in a CO2/EtOH bath, and a solution of 8 g (68.2 mmol) of 2-methoxy-N,N-dimethylacetamide in THF was added, the thickened reaction material was diluted with more THF and allowed to thaw, ethyl acetate, aq. citric acid, dil. aqueous sodium hydroxide solution to pH=6, aq. NaCl were added, the aqueous phase was extracted three times with ethyl acetate and the combined organic phases were dried with MgSO4 and concentrated by evaporation. The residue was distilled under reduced pressure in a kugelrohr and the distillate was recrystallized from a little benzotrifluoride. The temperature of the mixture increased cooled in a CO2/EtOH bath were added the aqueous phase was extracted three times with ethyl acetate the combined organic phases were dried with MgSO4 concentrated by evaporation The residue was distilled under reduced pressure in a kugelrohr the distillate was recrystallized from a little benzotrifluoride