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)