2-(二甲氨基)戊酸

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) Dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (11.1 mmol) 6-methylamino-2,3-dimethoxybenzamide dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 2 h and stirred overnight at room temperature. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum. The remaining thionyl chloride was distilled in vacuum The mixture was boiled for 2 h stirred overnight at room temperature After filtration the residue was dissolved in trichloromethane The organic solution was dried over magnesium sulfate evaporated under vacuum

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (9.51 mmol) 4,5-Dimethoxy-2-methylamino-benzamide (see above) dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 4 h. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum. The remaining thionyl chloride was distilled in vacuum The mixture was boiled for 4 h After filtration the residue was dissolved in trichloromethane The organic solution was dried over magnesium sulfate evaporated under vacuum

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (9.51 mmol) 4,5-Dimethoxy-2-methylamino-benzamide (see above) dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 4 h. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum. The remaining thionyl chloride was distilled in vacuum The mixture was boiled for 4 h After filtration the residue was dissolved in trichloromethane The organic solution was dried over magnesium sulfate evaporated under vacuum

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (9.42 mmol) 2-phenylamino-benzamide (see above) in 30 ml trichloromethane at 0° C. The reaction mixture was boiled for 4 h and stirred overnight at room temperature. The residue was filtrated and dissolved in dichloromethane and saturated sodium bicarbonate solution. The organic solvent was dried over magnesium sulfate and evaporated. The yellow oil slowly crystallized. The remaining thionyl chloride was distilled in vacuum The reaction mixture was boiled for 4 h stirred overnight at room temperature The residue was filtrated dissolved in dichloromethane The organic solvent was dried over magnesium sulfate evaporated The yellow oil slowly crystallized

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) Dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (11.1 mmol) 6-methylamino-2,3-dimethoxybenzamide dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 2 h and stirred overnight at room temperature. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum. The remaining thionyl chloride was distilled in vacuum The mixture was boiled for 2 h stirred overnight at room temperature After filtration the residue was dissolved in trichloromethane The organic solution was dried over magnesium sulfate evaporated under vacuum

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (9.51 mmol) 4,5-Dimethoxy-2-methylamino-benzamide (see above) dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 4 h. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum. The remaining thionyl chloride was distilled in vacuum The mixture was boiled for 4 h After filtration the residue was dissolved in trichloromethane The organic solution was dried over magnesium sulfate evaporated under vacuum

反应条件: temp:57.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.80 g (20.9 mmol) dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (9.42 mmol) 2-phenylamino-benzamide (see above) in 30 ml trichloromethane at 0° C. The reaction mixture was boiled for 4 h and stirred overnight at room temperature. The residue was filtrated and dissolved in dichloromethane and saturated sodium bicarbonate solution. The organic solvent was dried over magnesium sulfate and evaporated. The yellow oil slowly crystallized. The remaining thionyl chloride was distilled in vacuum The reaction mixture was boiled for 4 h stirred overnight at room temperature The residue was filtrated dissolved in dichloromethane The organic solvent was dried over magnesium sulfate evaporated The yellow oil slowly crystallized