Multi-Functional Chemical Agents, and the Method for Protein Modification
a chemical agent and multi-functional technology, applied in the field of biotechnology, can solve the problems of a huge limitation of engineered proteins, the difficulty of developing synthetic parallels of natural systems, and the difficulty of precise labeling of native proteins,
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example 1
General Procedures
[0120]The reagents, proteins, and enzymes were purchased from Sigma-Aldrich, Alfa Aeser and Merck Novabiochem. The organic solvents used were reagent grade. Aqueous buffers were prepared freshly using Millipore Grade I water (Resistivity>5 MΩ cm, Conductivity<0.2 μS / cm, TOC<30 ppb). Mettler Toledo (FE20) pH meter was used to adjust the final pH. The reaction mixture for the small molecules was stirred (Heidolph, 500-600 rpm). Proteins were either vortexed or incubated in incubator-shaker Thermo Scientific MaxQ 8000 (350 rpm, 25-37° C.). Cellulose membrane (MWCO, 6-8 kD) from Spectrum labs was used for dialysis. Amicon® Ultra-0.5 mL 3-kDa MWCO Centrifugal Filters from Merck Millipore was used to remove small molecules from protein mixture, desalting and buffer exchange. Organic solvents were removed by BUCHI rotavapor R-210 / 215 whereas aqueous samples were lyophilized by CHRiST ALPHA 2-4 LD plus lyophilizer. Circular Dichroism (CD) measurements were recorded on JASC...
example 2
Procedures for Synthesis of Multifunctional Chemical Agents and Characterization Data
[0124]Following reagents represent Class 2 (A). For the synthesis of the reagents of other classes, condensation of respective Fn1 and Fn2 using similar protocol and linkers are followed.
example 2a
Synthesis of 2-hydroxy-4-(oxiran-2-ylmethoxy)benzaldehyde (24)
[0125]
[0126]In 5 ml round bottom flask, 2,4-dihydroxybenzaldehyde (138 mg, 1 mmol) and K2CO3 (138 mg, 1 mmol) were dissolved in dry DMF (1 ml). To this solution, epibromohydrin (86 μl, 1 mmol) was added and stirred at room temperature. After 8 h, reaction mixture was carried out for ethylacetate:n-hexane (30:70) and water work up. The collected organic layers were dried with anh. sodium sulphate, filtered and concentrated in vacuo. The residue was purified by flash column chromatography using ethyl acetate:n-hexane (3:97) to give 24 (68 mg, 35% yield). 1H NMR (400 MHz, CDCl3) δ 11.45 (s, 1H), 9.73 (s, 1H), 7.44 (d, J=8.7 Hz, 1H), 6.57 (dd, J=8.7, 2.3 Hz, 1H), 6.43 (d, J=2.2 Hz, 1H), 4.31 (dd, J=11.1, 2.9 Hz, 1H), 3.97 (dd, J=11.1, 5.9 Hz, 1H), 3.41-3.32 (m, 1H), 2.93 (t, J=4.5 Hz, 1H), 2.76 (dd, J=4.8, 2.6 Hz, 1H). 13C NMR (101 MHz, CDCl3) δ 194.6, 165.6, 164.6, 135.5, 115.7, 108.8, 101.5, 69.2, 49.8, 44.7. HRMS (ESI) [MH...
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