A microwave-assisted method for preparing polypeptides
A microwave-assisted, polypeptide technology, which is applied in the field of microwave-assisted polypeptide preparation, can solve the problems of long polymerization reaction time, complicated and cumbersome operation, and low conversion rate of monomers, and achieve high industrial application value, simple experimental conditions, The effect of speeding up the reaction rate
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Embodiment 1
[0048] S1. Preparation of S-ethoxythiolthioglycolic acid (XAA)
[0049] Sodium hydroxide (10.0g, 25.0mmol) was first dissolved in ice-cold deionized water (250mL), then chloroacetic acid (23.62g, 25.0mmol) was added and stirred to obtain a clear solution, and potassium ethyl xanthate (40.1g , 25.0mmol) was added to the above solution. The mixture was stirred at room temperature for 24 h, then it was acidified to pH=1 with 4M aqueous hydrochloric acid. The resulting cloudy mixture was extracted with chloroform (3 x 200 mL), the combined organic extracts were dried over anhydrous magnesium sulfate for 24 h, filtered and concentrated in vacuo. n-Hexane (500 mL) was then added to the oily concentrate with vigorous stirring to give an off-white solid. The solid was collected by filtration, washed with a small amount of n-hexane, and dried under vacuum at room temperature for 24 h. The obtained white solid was the final product.
[0050] S2. Preparation of N(ε)-benzyloxycarbonyl-...
Embodiment 2
[0057] S1. Preparation of S-ethoxythiolthioglycolic acid (XAA): Same as Example 1.
[0058] S2. Preparation of N(ε)-benzyloxycarbonyl-D,L-lysine-N-thiocarboxylic anhydride (Lys-NTA): Same as Example 1.
[0059] S3. Configuration of hexamethylenediamine solution: same as in Example 1.
[0060] S4. Preparation of polylysine (PLys) by microwave-assisted method
[0061] Weigh Lys-NTA (48.32mg, 0.15mmol) into a 0.2-0.5mL microwave reaction tube, add 200μL of chloroform solution to dissolve it completely, and then add initiator hexamethylenediamine solution (40.8μL, 0.001875mmol, 76.6mM ), and finally add 59.2 μL of chloroform. The molar ratio of Lys-NTA to hexamethylenediamine in the final reaction system was 80:1, and the concentration of Lys-NTA was 0.5M. The microwave reaction tube was sealed and placed in a microwave reactor with a reaction temperature of 100° C. and a reaction time of 3 h. After the reaction was completed, the reaction liquid was added dropwise into diethy...
Embodiment 3
[0063] S1. Preparation of S-ethoxythiolthioglycolic acid (XAA): Same as Example 1.
[0064] S2. Preparation of N(ε)-benzyloxycarbonyl-D, L-lysine-N-thiocarboxylic anhydride (Lys-NTA): Same as Example 1.
[0065] S3. Configuration of hexamethylenediamine solution: same as in Example 1.
[0066] S4. Preparation of polylysine (PLys) by microwave-assisted method
[0067] Weigh Lys-NTA (48.32mg, 0.15mmol) and place it in a 0.2-0.5mL microwave reaction tube, add 200μL chloroform solution to dissolve it completely, then add initiator hexamethylenediamine solution (40.8μL, 0.001875mmol, 76.6 mM), and finally add 59.2 μL of chloroform. The molar ratio of Lys-NTA to hexamethylenediamine in the final reaction system was 80:1, and the concentration of Lys-NTA was 0.5M. The microwave reaction tube was sealed and placed in a microwave reactor with a reaction temperature of 120° C. and a reaction time of 2 h. After the reaction was completed, the reaction liquid was added dropwise into d...
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