A method for synthesizing sucralose-6-ethyl ester

Abstract

The invention relates to a method for synthesizing sucralose-6-ethyl ester. Its technical scheme includes the following production steps: 38.4 parts of sucrose-6-ethyl ester, 260.0 parts of N,N-dimethylformamide, 0.35 parts of zero-valent copper carbene as catalyst, 46.2 parts of carbon tetrachloride, aluminum Mix 5.4 parts of powder in proportion and add to the autoclave, then react at room temperature~50°C for 3 hours, then continue to react at 50~80°C for 3 hours, and finally react at 80~120°C for another 3 hours to obtain trichloro Sucrose‑6‑ethyl ester solution. Beneficial effect is: the present invention adopts low toxicity, non-corrosive carbon tetrachloride as the chlorination reagent of sucrose-6-ethyl ester chlorination; Simultaneously, the catalytic method used in the present invention is unique, uses carbene copper as catalyst , to catalyze the transfer of chlorine atoms on carbon tetrachloride to sucrose-6-ethyl ester, while using aluminum or zinc powder as a catalyst regeneration agent to regenerate the catalyst in situ, so that the chlorination of carbon tetrachloride as a chlorination agent The reaction can be carried out efficiently, greatly reducing the use of chlorinating agents.

Description

technical field [0001] The invention relates to a method for preparing a synthetic sweetener intermediate, in particular to a method for synthesizing sucralose-6-ethyl ester. Background technique [0002] Sucralose (CAS No.: 56038-13-2) is a new type of sweetener, which has the advantages of high sweetness (about 600 times that of sucrose), easily soluble in water, low calorie, and hardly absorbed by the human body. , the market prospect is very broad. At present, the method of industrially synthesizing sucralose is as follows: using sucrose as raw material, sucrose is subjected to esterification reaction to obtain sucrose-6-ethyl ester, and then chlorinated sucrose-6-ethyl ester to obtain sucralose-6-ethyl ester , and finally degreasing sucralose-6-ethyl ester to obtain sucralose. [0003] Among the three steps in the production of sucralose in the existing process, the chlorination of sucralose-6-ethyl ester to prepare sucralose-6-ethyl ester is the most difficult and pr...

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Problems solved by technology

但这些方法存在如下共同的缺陷:(1)反应需使用远过量的氯化试剂,如WO2008150379A1,WO2008096928A1,CN102964397A,CN102816188A,CN102417526A,CN101812095A,CN101768193A,CN101759728A,CN101619083B,CN101239997A,CN101239997A,CN101121736A,CN1962675A,CN1800194A The chlorination reagents used in the methods of patents such as these are often in excess of several times; (2) the chlorination reagents used are all highly toxic or corrosive, such as WO2008150379A1, WO2008096928A1, US2008103298A1, CN104387427A, CN103087116A, CN102417526A, CN1016318178A, CN437 Phosgene, solid phosgene, phosphorus trichloride, and phosphorus pentachloride used in patents such as CN1896087A, CN1660868A, and WO9960006A1 all have high toxicity, while thionyl chloride, phosphorus trichloride, and phosphorus pentachloride are all easy to form highly corrosive substances

Patents such as US2008300401A1, WO2007072496A2, CN101654467A, CN1911950A, and CN101125869A report the method for preparing sucralose-6-ethyl ester using triphenylchloromethane as a chlorination reagent. Although the method uses a low-toxicity chlorination reagent and chlorine The molar dosage of the chlorination reagent is relatively low, but triphenylchloromethane is expensive and has a large molecular weight (causing a high actual mass consumption of the chlorination reagent), which makes the raw material cost of this method higher

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