A kind of ionic liquid for synthesizing long-chain alkyl glycoside, its preparation method and application
A long-chain alkyl glycoside and ionic liquid technology, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of high viscosity of materials, inability to filter and separate ionic liquid catalysts, etc. The effect of mild reaction conditions and high conversion rate of glucose
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Embodiment 1
[0019] (1) Preparation of ionic liquid catalyst
[0020] Add equimolar 1,3-propane sultone and 1-butylimidazole into the three-necked flask, stir at 40°C for 10 h, and a white precipitate forms. After the reaction is complete, wash with ether three times, filter with suction, and dry in vacuo to obtain a white powder of 1-(butyl 4-sulfonic acid)-3-butylimidazolium salt (recovered ether is reused after distillation and purification). Add sulfuric acid and 1,3-propane sultone equimolar to the salt dropwise at room temperature, stir at 80°C for 6 hours, and dry in vacuum to obtain a transparent viscous ionic liquid. The structure of the ionic liquid is as follows:
[0021]
[0022] (2) Preparation of Alkyl Glycosides
[0023] Anhydrous glucose and isooctyl alcohol are added in the reactor in a molar ratio of 1:2, and the catalyst prepared in step (1) is added (the addition amount is 0.5% of the total mass of anhydrous glucose and alkyl alcohol) and the temperature is raised ...
Embodiment 2
[0025] (1) Preparation of ionic liquid catalyst
[0026] Add equimolar 1,3-propane sultone and 1-butylimidazole into the three-necked flask, stir at 50°C for 12h, and a white precipitate is formed. After the reaction is complete, wash with ether three times, filter with suction, and dry in vacuo to obtain a white powder of 1-(butyl 4-sulfonic acid)-3-butylimidazolium salt (recovered ether is reused after distillation and purification). Phosphoric acid and 1,3-propane sultone equimolar were added dropwise to the salt at room temperature, stirred at 80°C for 9 hours, and dried in vacuum to obtain a transparent viscous ionic liquid. The structure of the ionic liquid is as follows:
[0027]
[0028] (2) Preparation of Alkyl Glycosides
[0029] Anhydrous glucose and 2-propyl heptanol are added in the reactor in a molar ratio of 1: 6, and the catalyst (addition amount is 0.8% of the total mass of anhydrous glucose and alkyl alcohol) is added and the temperature is raised to Re...
Embodiment 3
[0031] (1) Preparation of ionic liquid catalyst
[0032] Add equimolar 1,3-propane sultone and 1-butylimidazole into the three-necked flask, stir at 45°C for 11 hours, and a white precipitate is formed. After the reaction is complete, wash with ether three times, filter with suction, and dry in vacuo to obtain a white powder of 1-(butyl 4-sulfonic acid)-3-butylimidazolium salt (recovered ether is reused after distillation and purification). Add p-toluenesulfonic acid and 1,3-propane sultone equimolar p-toluenesulfonic acid in batches slowly to the salt at room temperature and stir, react at 90°C for 9 hours, and dry in vacuum to obtain a transparent viscous ionic liquid. The structure of the ionic liquid is as follows:
[0033]
[0034] (2) Preparation of Alkyl Glycosides
[0035] Add anhydrous glucose and n-decyl alcohol into the reactor at a molar ratio of 1:8, add the catalyst prepared in step (1) (addition amount is 1% of the total mass of anhydrous glucose and alkyl ...
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