preparation | thermometer, dropping funnel and condenser tube are respectively installed on a 100ml dry three-diameter round bottom flask, 6-azelo [2.5] octane -1-carboxylic acid and acetone are sequentially added, and stirred at 35 ℃ for 30 minutes.. The reaction system is cooled to -10 ℃ in an ice salt bath, sodium hydroxide aqueous solution is added and stirred. When the reaction temperature drops to -5 ℃, di-tert-butyl dicarbonate is slowly added, and the temperature of the system is controlled to 0 ℃. After dropping for about 40 minutes, continue stirring for 1 hour. Wash the reaction solution to neutral, dry with anhydrous magnesium sulfate, evaporate the solvent, and recrystallize the solid with ethyl acetate /petroleum ether to obtain the product 6-(tert-butoxycarbonyl)-6-Azasol [2.5] octane -1-carboxylic acid. |