A kind of low cleaning residue magnetic beads and preparation method thereof
A magnetic bead and reaction technology, which is applied in the preparation methods of peptides, the preparation of carboxylate esters, chemical instruments and methods, etc., can solve the problems of difficult cleaning and other problems, and achieve the effects of low cleaning residues, reducing residues, and easy washing away.
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[0034] At the same time, the present invention provides a preparation method of low-cleaning residual magnetic beads, which comprises the preparation steps:
[0035] 1) Preparation of activated ester mixture
[0036] Put 5-(4,4'-dimethoxytriphenylmethoxy)-pentanoic acid and 4-pentynoic acid in a reaction tube, add dicyclohexylcarbodiimide and N-hydroxysuccinyl imine and DMF react at room temperature to obtain a mixture of activated esters, wherein the 5-(4,4'-dimethoxytriphenylmethoxy)-pentanoic acid, 4-pentynoic acid, di The mass volume ratio of cyclohexylcarbodiimide, N-hydroxysuccinimide and DMF is 50mg:25mg:25mg:13mg:1mL
[0037] 2) The surface of the magnetic beads is modified with hydroxyl and alkynyl groups
[0038] Add the activated ester mixture prepared in step 1) to the amino magnetic beads, shake the reaction at room temperature, and then add a DMF solution with a mass percentage of 10% TFA to obtain the magnetic beads with hydroxyl and alkynyl surface modificati...
Embodiment 1
[0048]19.3 g of benzyl 5-hydroxyvalerate was added to the reaction flask under argon protection, 100 mL of pyridine was added to the reaction flask, and the solid was completely dissolved by stirring; 37.7 g of 4,4'-dimethoxytris Phenylchloromethane (DMT-Cl), 0.2 g 4-dimethylaminopyridine (DMAP), keep the reaction at room temperature for 16 h, TLC monitoring the raw material reaction is complete; 10 mL methanol is added to quench the reaction, and the solvent is removed under reduced pressure at 40 °C; Add 150 mL of ethyl acetate and 100 mL of saturated aqueous sodium bicarbonate solution to separate the organic phase; wash the organic phase with saturated brine; add anhydrous sodium sulfate to dry the organic phase; through flash column chromatography PE:EA= After 30:1-20:1 separation, 13.0 g of product was obtained.
[0049] The structural formula of this product is:
[0050] .
[0051] 13.0 g of the product obtained in the previous step, 200 mL of ethyl acetate and 6 mL...
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