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A technology for sucralose and sucrose, which is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of residue pollution, difficult preparation, and difficult to recover, and achieves low production cost and high yield. Effect
Inactive Publication Date: 2011-06-29
JIANGSU JUBANG PHARMA
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[0010] The purpose of the present invention is to address the shortcomings of the existing sucralose single-protection route production process, such as the difficulty in preparing the intermediate sucrose-6-acetate in the lipidation protection step, and the presence of the catalyst itself in the chlorination step. Provide a new method for the preparation of sucralose by producing difficult-to-remove by-products or catalysts that are expensive, use a large amount, are difficult to recycle, and residues pollute products.
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Embodiment 2
[0023] Sucrose 34.2g (0.1mol) DMF 200ml, warm up to complete dissolution, cool, add p-toluenesulfonic acid 0.5g and vinyl acetate 9.7g (0.112mol), stir at room temperature for 12 hours overnight. TLC showed that there was almost no sucrose, vinyl acetate and by-product acetaldehyde were removed under reduced pressure, pH was adjusted to 9-9.5 with tert-butylamine, the temperature was raised to 40°C and kept for 2 hours, DMF was evaporated under reduced pressure to obtain 52.8 g of syrup, and the measured sucrose- The content of 6-acetate is 64.5%, and the yield is 88.7%.
Embodiment 3
[0025] Sucrose 171g (0.5mol) DMF 1000ml, in a 2000ml four-neck bottle, heated to complete dissolution, cooled to room temperature, added 1.0g benzenesulfonic acid and vinyl acetate 48.60g (0.565mol), stirred at room temperature overnight, TLC showed almost no sucrose, Remove excess raw materials and by-products under reduced pressure, adjust the pH to 9-9.5 with tert-butylamine, raise the temperature at 40°C and keep for 2 hours, evaporate DMF under reduced pressure to obtain 267.8 g of syrup, and the content of sucrose-6-acetate was measured to be 62.7%. Yield 87.4%.
Embodiment 4
[0027] Sucrose 3.42g (0.01mol), DMF 30ml, heat up to dissolve, cool to room temperature, add toluene solution containing 0.1g of dibutyltin oxide chloride and 1.7g (0.0105mol) of isopropenyl benzoate, stir overnight or track hexyl sugar by TLC Basically disappear, remove acetone under reduced pressure, add tert-butylamine to adjust pH to 9~9.5, raise temperature at 40°C for 2 hours, evaporate DMF under reduced pressure, add 30ml of acetone, stir and reflux for 1 hour, filter, wash with a small amount of acetone, reduce Dry under pressure to obtain 4.3 g of sucrose-6-benzoate, with a content of 98.7% and a yield of 94.9%.
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Abstract
The invention relates to a preparation method for the food sweetener, triclosan sucrose, including the steps of making the sucrose-6-ester with the sucrose , the preparation of the 1', 4, 6' - triclosan 1', 4, 6'-3-deoxy half milk sugar-6-ester through the chloride reaction of the sucrose-6-ester and the step to make the triclosan sucrose through the doffing of the ester. The invention is characterized in that the preparation of the sucrose-6-ester is the reaction of the sucrose with the enolase ester in the DMF solvent with the acidic catalyst to get the sucrose-6-ester. The acidic catalyst is anyone of the benzene sulfonic acid, the p-toluenesulfonic acid, the one-chlorine two-butyl tin oxide. The enolase esterification reagents include the vinyl acetate ester, thebenzoic isopropylene ester. The chlorinated reaction uses the organic tertiary amine as the catalyst and is done under the condition of changing the polarity of the solvent. The collection rate of each reaction in the invention is high; the content of the acquired products reaches above 99 percent; the production cost is low; and the invention is suitable for the industrial production.
Description
technical field [0001] The invention relates to a preparation method of food sweetener-sucralose. Background technique [0002] The chemical name of sucralose is 1',4,6'-trichloro-1',4,6'-trideoxygalactosucrose, which is a new type of strong sweetener, which is characterized by high sweetness and is sucrose 600 times that of sucrose; the sweetness is pure, the taste is basically the same as that of sucrose; the performance is stable, and it is not easy to be damaged by harsh environments such as acid, alkali, and high temperature; it has a wide range of applications and can be used in almost all foods, and it is safe to use in food; Non-rodent, suitable for diabetics and dental patients. The chemical structural formula of sucralose is: [0003] [0004] The preparation technology of existing sucralose is basically carried out according to the following steps: [0005] Sucrose → esterification protection → selective chlorination → deprotection group → sucralose, wherein...
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