4-甲基-哌啶-1-基胺

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

实验步骤: 6.3 Grams of N-amino-4-methylpiperadine, 6.0 g of triethylamine and 120 ml of chloroform were charged in a flask equipped with a stirrer, a condenser and a calcium chloride drying tube and stirred with ice cooling. To the solution was slowly added dropwise 15.2 g of hexadecyl chloroformate. After completion of the addition, the temperature of the solution was returned to room temperature, followed by refluxing with heating for 0.5 hour. The reaction mixture was cooled to room temperature, washed with water, dried over anhydrous magnesium sulfate and, then, concentrated under reduced pressure. The residue was recrystallized from acetonitrile to obtain 16.8 g of the desired product. m.p. 92° C. equipped with a stirrer, a condenser and a calcium chloride drying tube After completion of the addition was returned to room temperature by refluxing with heating for 0.5 hour washed with water dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was recrystallized from acetonitrile

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

实验步骤: 3.4 ml of conc. hydrochloric acid are added to 10.1 g (34 mmol) of the compound from Example 2 and 11.6 g (102 mmol) of N-amino-4-methyl-piperidine in 100 ml of toluene AR and 50 ml of dimethylformamide and the mixture is boiled for 24 hours in a water separator. The mixture is cooled, diluted using 200 ml of ethyl acetate and extracted three times using 1N hydrochloric acid and twice using saturated sodium hydrogen carbonate solution. The organic phase is dried over magnesium sulphate and concentrated in vacuo, and the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 5:95). The mixture is cooled diluted extracted three times The organic phase is dried over magnesium sulphate concentrated in vacuo the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 5:95)

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

实验步骤: 6.3 Grams of N-amino-4-methylpiperadine, 6.0 g of triethylamine and 120 ml of chloroform were charged in a flask equipped with a stirrer, a condenser and a calcium chloride drying tube and stirred with ice cooling. To the solution was slowly added dropwise 15.2 g of hexadecyl chloroformate. After completion of the addition, the temperature of the solution was returned to room temperature, followed by refluxing with heating for 0.5 hour. The reaction mixture was cooled to room temperature, washed with water, dried over anhydrous magnesium sulfate and, then, concentrated under reduced pressure. The residue was recrystallized from acetonitrile to obtain 16.8 g of the desired product. m.p. 92° C. equipped with a stirrer, a condenser and a calcium chloride drying tube After completion of the addition was returned to room temperature by refluxing with heating for 0.5 hour washed with water dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was recrystallized from acetonitrile

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

实验步骤: 3.4 ml of conc. hydrochloric acid are added to 10.1 g (34 mmol) of the compound from Example 2 and 11.6 g (102 mmol) of N-amino-4-methyl-piperidine in 100 ml of toluene AR and 50 ml of dimethylformamide and the mixture is boiled for 24 hours in a water separator. The mixture is cooled, diluted using 200 ml of ethyl acetate and extracted three times using 1N hydrochloric acid and twice using saturated sodium hydrogen carbonate solution. The organic phase is dried over magnesium sulphate and concentrated in vacuo, and the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 5:95). The mixture is cooled diluted extracted three times The organic phase is dried over magnesium sulphate concentrated in vacuo the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 5:95)

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

实验步骤: 6.3 Grams of N-amino-4-methylpiperadine, 6.0 g of triethylamine and 120 ml of chloroform were charged in a flask equipped with a stirrer, a condenser and a calcium chloride drying tube and stirred with ice cooling. To the solution was slowly added dropwise 15.2 g of hexadecyl chloroformate. After completion of the addition, the temperature of the solution was returned to room temperature, followed by refluxing with heating for 0.5 hour. The reaction mixture was cooled to room temperature, washed with water, dried over anhydrous magnesium sulfate and, then, concentrated under reduced pressure. The residue was recrystallized from acetonitrile to obtain 16.8 g of the desired product. m.p. 92° C. equipped with a stirrer, a condenser and a calcium chloride drying tube After completion of the addition was returned to room temperature by refluxing with heating for 0.5 hour washed with water dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was recrystallized from acetonitrile