A kind of purification method of sucrose-6-acetate
A purification method and an acetate technology are applied in the field of purification of sucrose-6-acetate, which can solve the problems of not too high purity, troublesome ion exchange resin processing, large amount of solvent, etc. The effect of large-scale industrial production and low equipment requirements
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Embodiment 1
[0020] A kind of purification method of sucrose-6-acetate, concrete steps are:
[0021] Remove most of the DMF from the DMF solution of sucrose-6-acetate under reduced pressure distillation to obtain the crude product of sucrose-6-acetate. Add isoamyl alcohol at 20°C, and a large amount of crystals are precipitated. Filtration, the precipitated crystals were dried in a vacuum oven, and the volume ratio of the used isoamyl alcohol to the crude product of sucrose-6-acetate was 3:1; 3.7 g of sucrose-6-acetate was obtained with a yield of 82%. The product was analyzed by phase chromatography, and the purity of sucrose-6-acetate was 92%.
[0022] Wherein, according to liquid chromatography, referring to the reference document US4889928, the sucrose-6-acetate is confirmed according to the retention time, and its content value is obtained according to the peak area ratio. Specific conditions are as follows: Zorbax NH 2 Column, mobile phase is V (water): V (acetonitrile) = 85:15, fl...
Embodiment 2
[0024] A kind of purification method of sucrose-6-acetate, concrete steps are:
[0025] Remove most of the DMF from the DMF solution of sucrose-6-acetate under reduced pressure distillation to obtain the crude product of sucrose-6-acetate. Add isoamyl alcohol at 20°C, and a large amount of crystals are precipitated. Filtration, the precipitated crystals were dried in a vacuum oven, the volume ratio of the used isoamyl alcohol to the crude product of sucrose-6-acetate was 2:1; 3.6g of sucrose-6-acetate was obtained, the yield was 80%, and the liquid The product was analyzed by phase chromatography, and the purity of sucrose-6-acetate was 90%.
Embodiment 3
[0027] A kind of purification method of sucrose-6-acetate, concrete steps are:
[0028] Remove most of the DMF from the DMF solution of sucrose-6-acetate under vacuum distillation to obtain the crude product of sucrose-6-acetate. Add isoamyl alcohol at 30°C, and a large amount of crystals are precipitated. Filtration, the precipitated crystals were dried in a vacuum oven, and the volume ratio of the used isoamyl alcohol to the crude sucrose-6-acetate was 2:1; 3.4 g of sucrose-6-acetate was obtained, with a yield of 76%. The product was analyzed by phase chromatography, and the purity of sucrose-6-acetate was 80%. The solubility of sucrose-6-acetate in isoamyl alcohol increases with increasing temperature.
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