Methods and reagents for preparing peptide/protein conjugates
A protein and compound technology, applied in the preparation method of peptide, animal/human protein, anti-animal/human immunoglobulin, etc., can solve the problem of cell toxicity
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[0029] The present invention relates to a preparation method of compound (1) represented by formula (1),
[0030]
[0031] wherein R' represents a substituent, and R represents H or at least one substituent.
[0032] The compound (1) is produced by reacting the compound (2) represented by the formula (2) with the compound (3) represented by the formula (3).
[0033] R'-NH 2 (2)
[0034]
[0035] In the above formula, R' can be any substituent, especially a peptide residue and / or a protein residue. The peptide residues may be synthetic or natural peptide residues. The protein residues may be natural protein residues or recombinant protein residues, or enzyme residues or antibody residues. The peptide residues may have at least one lysine residue in the sequence. R can be any substituent, preferably selected from alkyl, epoxide, amide, amine, ketone, aldehyde, phosphate, sulfate, halide, nitrile, nitro, azido , thiol group, carboxylic acid group, alkynyl group, este...
Embodiment 1
[0047] Will NH 2 CH 2 CH 2 NHBoc was dissolved in PBS buffer (pH=7.4) at a concentration of 1 mM, and compound 2 (1.2 equivalents) was added. The reaction mixture was stirred at room temperature for 1 hour. The product (%) was isolated using chromatography. 1 H NMR (CDCl 3 )δ7.30(2H,m),7.05(1H,m),5.02(1H,s),4.30(2H,s),3.84(3H,s),3.80(2H,m),3.38(2H,m ),1.28(9H,s); 13 C NMR (CDCl 3 )δ170.8,161.4,157.6,135.2,134.9,125.0,121.2,107.8,80.9,57.1,51.5,43.9,40.8,29.8.( figure 2 )
Embodiment 2
[0049] As a model study, the peptide Ac-AKLHA-OH was prepared by solid-phase peptide synthesis. A typical procedure for OPA / amine conjugation is as follows: Compound 1 is added to a solution of lysine-containing peptide in PBS buffer (pH=7.4) at a concentration of 0.01 mM. The reaction mixture was stirred at room temperature. The progress of the reaction is monitored by measuring the change in fluorescence. The fluorescence intensity increased with time and reached a maximum at 10 min ( image 3 ). The product was analyzed by LC-MS ( Figure 4 ). Ac-AKPHA-OH, ESI-MS, calculated M+H+: 546.4, measured 564; product ESI-MS, calculated M+H+: 680.3, measured 680.1.
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