Preparation method for nonyl glucoside
A technology of nonyl glucoside and fully acylated nonyl glucoside is applied in the field of preparation of nonyl glucoside, can solve the problems of difficult separation of product and catalyst, deepened product color, complicated operation steps and the like, and achieves low production cost, Easy operation and simple process effect
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Embodiment 1
[0017] a. Synthesis of fully acylated nonyl glycosides
[0018] Mix 1g of fully acetylated mannose with 3.0ml of nonanol (Acros) and 30ml of anhydrous toluene, stir and add 1.0mL of boron trifluoride ether (chemically pure) at room temperature, then heat to 50°C and continue stirring to carry out the per-acyl The reaction was carried out for 5 hours, and after the reaction was completed, the pure white solid was separated by column chromatography, which was fully acylated nonyl mannoside, and the yield was 36% (α:β>19:1).
[0019] The NMR structure analysis of fully acylated nonyl glucoside was carried out, and the test data are as follows:
[0020] 1 H NMR (500MHz, CDCl 3 ), δ: 0.92(t, 3H, CH 3 ), 1.30-1.37(m, 12H), 1.62-1.65(m, 2H), 2.03, 2.08, 2.14, 2.19(s, 12H, 4COCH 3 ), 3.48(m, 1H), 3.70(m, 1H), 3.71(m, 1H), 4.01(m, 1H), , 4.15(m, 1H), 4.31(m, 1H), 4.83(br s 1H ), 5.27(br s 1H), 5.31(m, 1H), 5.39(m, 1H)
[0021] b. Synthesis of Nonyl Glycosides
[0022] Take 0.25 ...
Embodiment 2
[0029] a. Synthesis of fully acylated nonyl glycosides
[0030] Take 5g of fully acetylated xylose, mix with 10.0ml of nonanol (Acros) and 250ml of anhydrous dichloromethane, stir and add 1.0mL of trimethylsilyl trifluoromethanesulfonate (TMSOTf) (Aldrich) at 0°C, Then be warmed to 25 ℃ and continue to stir, carry out full acylation reaction 3 hours, obtain pure white solid through column chromatography separation after reaction is full acylation nonyl xyloside, and its productive rate is 42% (α: β ~1.7:1).
[0031] b. Synthesis of Nonyl Glycosides
[0032] Take 2 g of the above-mentioned product fully acylated nonyl xyloside and add 5 ml of absolute ethanol to mix, stir and slowly add 0.1 g of NaOH dropwise at room temperature, carry out the deacylation reaction for 1 hour, and add dropwise 732 type ion exchange resin ( h + , ~ 6g) neutralized to pH=7, then filtered, and the filtrate was suspended and evaporated under reduced pressure to remove the solvent, and obtained wh...
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