A polyethylene glycol conjugate of teduglutide and its solid-phase preparation method
A technology of solid-phase preparation and polyethylene glycol, which is applied in the preparation method of peptides, chemical instruments and methods, peptides, etc., can solve the problems of wide Mr distribution of protein molecules, immunogenicity, short half-life, etc.
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Embodiment 1
[0040] Embodiment 1: the synthesis of the Fmoc-Asp(OtBu)-Wang resin that substitution degree is 0.1mmol / g
[0041] Weigh 40 g of Wang resin with a substitution degree of 1.0 mmol / g, add it to a solid-phase reaction column, wash it twice with DMF, and swell the resin with DMF for 30 minutes. Weigh 4.94g Fmoc-Asp(OtBu)-OH (12mmol), 1.95g HOBt (14.4mmol) and 0.15g DMAP (1.2mmol) and dissolve in the mixed solution of DCM and DMF with a volume ratio of 1:1, add 2.25ml of DIC (14.4mmol) was activated for 3 minutes and then added to the solid-phase reaction column, and reacted at room temperature for 2 hours. Wash 3 times with DMF, add 70ml of blocking solution (pyridine / acetic anhydride = 1:1, 400mmol: 400mmol) to block for 8 hours (if the resin is not fully diffused, add DCM as a solvent). Wash 4 times with DMF, 4 times with DCM, shrink and dry with methanol to obtain Fmoc-Asp(OtBu)-Wang resin. The detected substitution degree was 0.098mmol / g.
Embodiment 2
[0042] Embodiment 2: the degree of substitution is the synthesis of Fmoc-Asp(OtBu)-Wang resin of 0.19mmol / g
[0043] Weigh 40 g of Wang resin with a substitution degree of 1.0 mmol / g, add it to a solid-phase reaction column, wash it twice with DMF, and swell the resin with DMF for 30 minutes. Weigh 9.38g Fmoc-Asp(OtBu)-OH (22.8mmol), 3.70g HOBt (27.4mmol) and 0.28g DMAP (0.23mmol) and dissolve them in a mixed solution of DCM and DMF with a volume ratio of 1:1. Add 4.28ml DIC (27.4mmol) to activate for 3 minutes, then add to the solid phase reaction column, and react at room temperature for 2 hours. Wash 3 times with DMF, add 70ml of blocking solution (pyridine / acetic anhydride = 1:1, 400mmol: 400mmol) to block for 8 hours (if the resin is not fully diffused, add DCM as a solvent). Wash 4 times with DMF, 4 times with DCM, shrink and dry with methanol to obtain Fmoc-Asp(OtBu)-Wang resin. The detected substitution degree was 0.192mmol / g.
Embodiment 3
[0044] Embodiment 3: the degree of substitution is the synthesis of Fmoc-Asp(OtBu)-Wang resin of 0.15mmol / g
[0045] Weigh 40 g of Wang resin with a substitution degree of 1.0 mmol / g, add it to a solid-phase reaction column, wash it twice with DMF, and swell the resin with DMF for 30 minutes. Weigh 7.42g Fmoc-Asp(OtBu)-OH (18mmol), 2.92g HOBt (21.6mmol) and 0.22g DMAP (1.8mmol) and dissolve in the mixed solution of DCM and DMF with a volume ratio of 1:1, add 3.38ml DIC (21.6mmol) was activated for 3 minutes and then added to the solid-phase reaction column, and reacted at room temperature for 2 hours. Wash 3 times with DMF, add 70ml of blocking solution (pyridine / acetic anhydride = 1:1, 400mmol: 400mmol) to block for 8 hours (if the resin is not fully diffused, add DCM as a solvent). Wash 4 times with DMF, 4 times with DCM, shrink and dry with methanol to obtain Fmoc-Asp(OtBu)-Wang resin. The detection substitution degree was 0.150mmol / g.
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