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    • 1. 发明申请
    • METHOD FOR THE PREPARATION OF OLIGOCARBAMATES WITH A DEFINED MONOMERIC SEQUENCE
    • WO2022112868A1
    • 2022-06-02
    • PCT/IB2021/057872
    • 2021-08-27
    • SIEĆ BADAWCZA ŁUKASIEWICZ – PORT POLSKI OŚRODEK ROZWOJU TECHNOLOGII
    • SZWEDA, RóżaWALENCIK, Paulina KatarzynaTURSKI, Mateusz BolesławCWYNAR, Paweł
    • C07C269/06C07C271/16
    • The subject matter of the invention is a method for the preparation of oligocarbamates with a defined monomeric sequence of the general formula (I) characterised in that the multistage synthesis is performed in one reaction pot without the necessity for purification between successive reactions, and the synthesis is driven by the addition of fresh portions of the Ν,Ν'-disuccinimidyl carbonate activator or a monomer in the form of HO-R2-NH2 aminoalcohol, after complete conversion of the previous step has been confirmed, the method comprising the following steps: i. initiation which comprises the activation of 1 equiv. of alcohol dissolved in dry acetonitrile - a solution of 0.1-1 M with 3-12 equiv. of dry pyridine added -by the addition of an activator, being 1.2-2.1 equiv. of Ν,Ν'-disuccinimidyl carbonate, to the mixture and performing the reaction at room temperature until complete activation of alcohol, wherein the R1-OH alcohol is an aromatic primary or secondary alcohol not containing free nucleophilic groups in its structure; (ii.) at least one propagation of the oligomer chain by the addition of a portion of 1-2 equiv. of the first monomer in the form of HO-R 2-NH2 alcohol to 1 equiv. of the activated alcohol of step (i.) and performing the reaction until complete conversion of the activated alcohol, and then the addition of a further portion of the activator, being 1.2-2.1 equiv. of Ν,Ν'-disuccinimidyl carbonate, to activate the hydroxyl group of the growing macromolecule, wherein the substituent R2 is selected from the group comprising a linear or branched C3-C8 alkyl and a C3-C8 alkyl having at least one aryl, composed of 3-8 carbon atoms and not containing free nucleophilic groups in its structure; (iii.) repeating the propagation step until the desired oligocarbamate sequence is achieved.