Preparation method with lauroyl aminoacyl proline methyl ester serving as novel chemical penetration enhancer and application
A technology of penetration enhancer and amino acid, applied in the field of biomedicine, can solve the problems of low transdermal absorption rate of drugs
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Embodiment 1
[0028] The preparation of embodiment 1Pro-OMe
[0029] In an ice bath, 1.3 mL of SOCl was added dropwise to 7.5 mL of methanol 2 , after reacting for 30 minutes, dissolve proline in methanol until the reaction is complete, drain the reaction solution under reduced pressure, add a small amount of methanol to dissolve, and drain under reduced pressure, repeat three times, then add anhydrous ether, and drain under reduced pressure dry, and repeat the same three times. Dissolve the treated product with a small amount of methanol, add anhydrous ether drop by drop until crystals precipitate, put it in the refrigerator overnight, filter the crystals to obtain proline methyl ester, and store it in the refrigerator for later use. White snowflake crystals (ESI-MS(m / z): 152.2[M+Na] + )
Embodiment 2C1
[0030] Example 2C 12 - Preparation of L-Gly-L-Pro-OMe
[0031] (1) Synthesis of Boc-Gly-OH
[0032] Under the condition of ice bath, put 0.75g (10mmol) glycine into an eggplant bottle, slowly add 10mL of 1N NaOH solution to completely dissolve the amino acid. In a small beaker 2.398g (11mmol) (Boc) 2 O, add 10mL of 1,4-dioxane to dissolve completely, then slowly add to the eggplant bottle, adjust the pH to 8-9 with NaOH solution, and the reaction is complete under ice bath conditions. Add saturated KHSO to the reaction solution 4 Adjust the pH to neutral, pressurize and concentrate to dryness to obtain a white solid, add a small amount of water to dissolve with saturated KHSO 4 Adjust to pH=2, and extract three times with ethyl acetate solution, combine the ethyl acetate layers, and extract three times with saturated NaCl. Ethyl acetate layer with anhydrous Na 2 SO 4 Dry overnight, filter to remove Na 2 SO 4 , the filtrate was concentrated to dryness under reduced pre...
Embodiment 3C1
[0040] Example 3C 12 - Preparation of L-Ala-L-Pro-OMe
[0041] (1) Synthesis of Boc-Ala-OH
[0042] Under the condition of ice bath, take 0.8909g (10mmol) alanine into the eggplant bottle, slowly add 10mL of 1N NaOH solution to completely dissolve the amino acid. In a small beaker 2.398g (11mmol) (Boc) 2 O, add 10mL of 1,4-dioxane to dissolve completely, then slowly add to the eggplant bottle, adjust the pH to 8-9 with NaOH solution, and the reaction is complete under ice bath conditions. Add saturated KHSO to the reaction solution 4 Adjust the pH to neutral, pressurize and concentrate to dryness to obtain a white solid, add a small amount of water to dissolve with saturated KHSO 4 Adjust to pH=2, and extract three times with ethyl acetate solution, combine the ethyl acetate layers, and extract three times with saturated NaCl. Ethyl acetate layer with anhydrous Na 2 SO 4 Dry overnight, filter to remove Na 2 SO 4 , the filtrate was concentrated to dryness under reduced...
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