Method for synthesizing sucrose-6-acetic ester
View Patent ↗The present invention discloses a method of synthesizing sucrose-6-acetic ester, comprising the following steps: adding sucrose into a polar aprotic solvent, and stirring the solvent to dissolve it, then generate a suspension solution of sucrose; adding a acetylation agent acetylnitrile into said suspension solution and stirring the solution; adding water into the aforesaid reaction solution, and then concentrating it to generate a concentrated product; adding a crystalline solvent into the concentrated product, stirring to dissolve it, and depositing for crystallization, then filtering and drying it to get a product of sucrose-6-acetic ester. The benefit of the present invention is that the method of synthesizing sucrose-6-acetic ester has simple operation, mild reaction condition, high selectivity, high yield, and is suitable for industrial production.
1. A method for synthesizing sucrose-6-acetic ester, consisting of the following steps:
(a) adding sucrose into a polar aprotic solvent and stirring the solvent to generate a suspension solution of sucrose, wherein said polar aprotic solvent is selected from the group consisting of: N,N-dimethylformamide, hexamethyl-phosphoric triamide, acetonitrile, and propionitrile;
(b) adding acetylnitrile into said suspension solution and stirring the solution at a reaction temperature of acetyInitrile and sucrose of 20° C.-60° C.;
(c) adding water into the reaction solution of step (b) and then concentrating it to generate a concentrated product; and
(d) adding crystallization solvent into the concentrated product, stirring to dissolve it, and depositing for crystallization, then filtering and drying it to get a product of sucrose-6-acetic ester.
2. The method for synthesizing sucrose-6-acetic ester as in claim 1 , wherein said acetylnitrile is obtained by reaction of diethoxy-phosphoryl cyanide dissolved in acetic acid.
3. The method for synthesizing sucrose-6-acetic ester as in claim 2 , wherein a reaction temperature of diethoxy-phosphoryl cyanide and acetic acid is 25° C.-35° C.
4. The method for synthesizing sucrose-6-acetic ester as in claim 2 or 3 , wherein said acetylnitrile obtained by the reaction of diethoxy-phosphoryl and acetic acid, is purified by distillation after the reaction.
5. The method for synthesizing sucrose-6-acetic ester as in claim 1 , wherein a mole proportion of acetyInitrile and sucrose is 0.8:1-3:1.
6. The method for synthesizing sucrose-6-acetic ester as in claim 1 , wherein in said step (d), said solvent is a component solvent of water and acetone.
7. The method for synthesizing sucrose-6-acetic ester as in claim 6 , wherein a proportion of water and acetone in said component solvent of water and acetone is 1:3-1:8.
8. The method for synthesizing sucrose-6-acetic ester as in claim 1 or 6 , wherein the temperature for crystallization is 10° C.-30° C.