Glucose ferulic amide and process for preparing same
A technology of ferulic acid amide and glucose, applied in the field of glucosamide, can solve the problem that derivatives have not been reported, and achieve the effects of promoting drug transdermal penetration activity, high drug transdermal penetration activity, and simple preparation process.
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Embodiment 1
[0024] Example 1: 2-deoxy-2-(m-methoxy-p-hydroxyphenylacrylamide)-β-D-glucopyranose
[0025] Step 1: Synthesis of N-(β-D-glucose) benzaldimine
[0026] Add glucosamine hydrochloride (46mmol, 10.0g) into an aqueous solution (47mL) containing NaOH (55mmol, 2.2g), and stir until completely dissolved. The solution was cooled down to 0°C, benzaldehyde (53mmol, 5.4mL) was slowly added under vigorous stirring, stirred for 1h and then left at 0°C for 12h. The mixture was then poured into an ice-water mixture and left standing at 0 °C for 1 h. A white precipitate was obtained by filtration, washed with anhydrous ether (60 mL×3), and dried to obtain a white solid (7.9 g, yield 63.7%).
[0027] Step 2: Synthesis of N-(1,3,4,6-tetra-O-acetyl-β-D-glucose) benzaldimine
[0028] Dissolve N-(β-D-glucose)benzaldimine (45mmol, 11.9g) in pyridine (70mL), add acetic anhydride (450mmol, 42mL) under stirring in an ice-water bath, stir in an ice-water bath for 30min, and then heat up Keep warm a...
Embodiment 2
[0035] Example 2: N-(β-D-glucose)-1-(m-methoxy-p-hexadecyloxyphenyl)acrylamide
[0036] Step 1, Step 2, Step 3, and Step 4 of this embodiment are the same as those of Embodiment 1.
[0037] Step 5: 1,3,4,6-tetra-O-acetyl-2-deoxy-2-(m-methoxy-p-hexadecyloxyphenylacrylamide)-β-D-glucopyranose Synthesis
[0038] 1,3,4,6-tetra-O-acetyl-2-deoxy-2-(m-methoxy-p-hydroxyphenylacrylamide)-β-D-glucopyranose (1mmol, 0.523g) Dissolve in N,N-dimethylformamide (10 mL), add sodium hydride (2 mmol, 0.053 g) and hexadecane bromide (1.5 mmol, 0.47 g), and stir at room temperature for 48 h. After evaporating to dryness under reduced pressure, the resulting solid was dissolved in dichloromethane (20 mL), washed with water (30 mL×8), dried over anhydrous sodium sulfate, concentrated, and purified on a silica gel column. The developing solvent is ethyl acetate:petroleum ether=3:2 (V:V). A white solid (0.384 g, yield 51.5%) was obtained. The melting point is 119-121°C. IR(KBr)Δ / cm-1: 3272, 2922...
Embodiment 3
[0041] Example 3: N-(β-D-glucose)-1-(m-methoxy-p-n-octyloxyphenyl)acrylamide
[0042] Step 1: Synthesis of N-(β-D-glucose) benzaldimine
[0043] Add glucosamine hydrochloride (46mmol, 10.0g) into an aqueous solution (47mL) containing NaOH (55mmol, 2.2g), and stir until completely dissolved. The solution was cooled down to 0°C, benzaldehyde (46mmol, 4.7mL) was slowly added under vigorous stirring, stirred for 1h and left at 0°C for 12h. The mixture was then poured into an ice-water mixture and left standing at 0 °C for 1 h. A white precipitate was obtained by filtration, washed with anhydrous ether (60 mL×3), and dried to obtain a white solid (7.3 g, yield 58.8%).
[0044] Step 2: Synthesis of N-(1,3,4,6-tetra-O-acetyl-β-D-glucose) benzaldimine
[0045] Dissolve N-(β-D-glucose)benzaldimine (38mmol, 10.0g) in pyridine (70mL), add acetic anhydride (364mmol, 36mL) under stirring in an ice-water bath, stir in an ice-water bath for 30min, and then heat up Keep warm at 35°C-40°C ...
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