Method for preparing sucralose-6-acetate
A technology of sucralose and acetate, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of high reaction temperature requirements, increased difficulty in operation, long reaction time, etc., and achieve the goal of "three wastes" Less, convenient post-processing, and simple process operation
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Embodiment 1
[0023] Preparation of Sulfonated Cage Mesoporous Carbon
[0024] Using F127 as the structure-directing agent and tetraethyl orthosilicate as the silicon source, after hydrothermal synthesis at 150°C, the structure-directing agent was calcined in a muffle furnace to obtain mesoporous silica KIT-5-150, which is characterized by ordered mesoporous Silicon KIT-5-150 is the silicon template, sucrose is the carbon source, and the sucrose is repeatedly poured into the silicon template twice, after thermal polymerization, a mesoscopic phase is formed, and then carbonized in a nitrogen atmosphere, and finally the silicon template is soaked in hydrofluoric acid , to obtain cage-type mesoporous carbon CKT-3 (A); CKT-3 (A), isoamyl nitrite and p-aminobenzenesulfonic acid were added to water, at 80 ° C and under stirring, with isoamyl nitrite and The sulfonic acid phenyl radical generated by the reaction of p-aminobenzenesulfonic acid reacted with the mesoporous carbon CKT-3(A) to achieve ...
Embodiment 2
[0030] The difference between this example and Example 1 lies in the preparation of the phthalate-based cationic gemini surfactant.
[0031] In 250 milliliters of three-necked round bottom flasks, add respectively dimethyl phthalate 58g (0.03mol), N, N-dimethylethanolamine 11g (0.12mol), the sulfonated bamboo charcoal catalyst 10g that embodiment 2 makes, The reaction was heated at 100°C for 5 hours, and methanol was continuously distilled out from the system. After 12 hours, it was changed to vacuum distillation to recover excess N,N-dimethylethanolamine. Cool to room temperature, add 60 ml of chlorohexane, reflux and stir for 24 hours, distill off the solvent, cool and solidify, and recrystallize from acetonitrile to obtain the product.
Embodiment 3
[0033] The difference between this example and Example 1 lies in the preparation of the phthalate-based cationic gemini surfactant.
[0034] In 250 milliliters of three-necked round bottom flasks, add respectively dimethyl phthalate 58g (0.03mol), N, N-dimethylethanolamine 11g (0.12mol), the sulfonated bamboo charcoal catalyst 10g that embodiment 3 makes, The reaction was heated at 100°C for 5 hours, and methanol was continuously distilled out from the system. After 12 hours, it was changed to vacuum distillation to recover excess N,N-dimethylethanolamine. Cool to room temperature, add 60 ml of benzyl chloride, reflux and stir for 24 hours, distill off the solvent, cool and solidify, and recrystallize from acetonitrile to obtain the product.
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