反应详情

Aqueous D-glucaric acid (1, ˜1 M, 4.51 mL) and aqueous octamethylenediamine (1 M, 5.94 mL) were mixed in a round bottom flask, and stirred at room temperature for 10 min. The reaction mixture was then stirred at 60° C. for 26 h and concentrated to less than 25% of the total volume. Methanol (6˜8 mL) was added drop-wise to the concentrated solution and the reaction mixture was stirred for 12 h. The top methanol phase was removed and the light amber syrup was washed with methanol (2×5 mL), and then dried under vacuum at room temperature for 24 h to give octamethylenediammonium D-glucarate (5a)/1 and 6-[N-(8-ammoniumooctyl)]-D-glucaramates (5b and 5c) (1.54 g, 4.35 mmol, 96.43%).

1. stirringThe reaction mixture was then stirred at 60° C. for 26 h
2. concentrationconcentrated to less than 25% of the total volume
3. additionMethanol (6˜8 mL) was added drop-wise to the concentrated solution
4. stirringthe reaction mixture was stirred for 12 h
5. customThe top methanol phase was removed
6. washthe light amber syrup was washed with methanol (2×5 mL)
7. customdried under vacuum at room temperature for 24 h