反应详情

3.5 g of 12-aminododecanoic acid are dissolved in 500 ml of methanol and, with 2.7 g of finely powdered sodium carbonate and 4.8 g of 3,4,5-trihydroxy-6-hydroxymethyltetrahydropyran-2-one, stirred at room temperature for 30 hours. The mixture is filtered off, the filtrate is concentrated and the residue is dissolved in 70 ml of water. With ice-cooling, 1N hydrochloric acid is added gradually until the pH is 1-2 (about 50-55 ml). The free acid precipitates out and is filtered off with suction, washed with a little cold water, and dried under high vacuum at 35° C. This gives 9 of molecular weight 393.48 (C18H35NO8); MS (ESI+): 394 (M+H+); (ESI−):392 (M−H)−.

1. filtrationThe mixture is filtered off
2. concentrationthe filtrate is concentrated
3. dissolutionthe residue is dissolved in 70 ml of water
4. temperatureWith ice-cooling
5. addition1N hydrochloric acid is added gradually until the pH is 1-2 (about 50-55 ml)
6. customThe free acid precipitates out
7. filtrationis filtered off with suction
8. washwashed with a little cold water
9. customdried under high vacuum at 35° C
10. customThis gives 9 of molecular weight 393.48 (C18H35NO8)