Preparation method of homocyclopeptide cyclo-(ala)4
A technology of cyclic peptide and resin, which is applied in the field of cyclic peptide compound cyclic peptide Cyclo-4 and its synthesis and preparation technology, to achieve good fat solubility and stability in vivo, high synthesis efficiency, good regularity and multi-directional symmetry.
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Embodiment 1
[0027] A homocyclic peptide Cyclo-(Ala) 4 preparation methods, including:
[0028]Step 1. Soak 2-chlorotrityl chloride resin with dichloromethane and shake for 30 minutes; remove the solvent after the resin is swollen, and take a three-fold molar excess of alanine with fluorenyl moxycarbonyl protecting group in the resin 1. N,N-diisopropylethylamine is added to the resin in a ten-fold molar excess, then DMF is added to dissolve it, and the reaction is shaken at room temperature for 30 minutes; then methanol is added to incubate for 20 minutes; the reactive sites on the resin are sealed; Wash the resin repeatedly with DMF and methanol solvent and remove the solvent. The first amino acid is connected to the resin; After fully washing with ethanol, add one drop each of 5% ninhydrin ethanol solution, 0.3% ascorbic acid solution, and 60% phenol solution, and heat to 110°C and keep it warm for 5 minutes. If the resin color turns dark blue, then It shows that the amino acid has bee...
Embodiment 2
[0033] A homocyclic peptide Cyclo-(Ala) 4 preparation methods, including:
[0034] Step 1. Soak 2-chlorotrityl chloride resin with dichloromethane and shake for 30 minutes; remove the solvent after the resin is swollen, and take a three-fold molar excess of alanine with fluorenyl moxycarbonyl protecting group in the resin 1. N,N-diisopropylethylamine is added to the resin in a ten-fold molar excess, then DMF is added to dissolve it, and the reaction is shaken at room temperature for 30 minutes; then methanol is added to incubate for 20 minutes; the reactive sites on the resin are sealed; Wash the resin repeatedly with DMF and methanol solvent and remove the solvent. The first amino acid is connected to the resin; After fully washing with ethanol, add one drop each of 5% ninhydrin ethanol solution, 0.3% ascorbic acid solution, and 60% phenol solution, and heat to 105°C for 5 minutes at the same time. If the resin color turns dark blue, then It shows that the amino acid has be...
Embodiment 3
[0039] A homocyclic peptide Cyclo-(Ala) 4 preparation methods, including:
[0040] Step 1. Soak 2-chlorotrityl chloride resin with dichloromethane and shake for 30 minutes; remove the solvent after the resin is swollen, and take a three-fold molar excess of alanine with fluorenyl moxycarbonyl protecting group in the resin 1. N,N-diisopropylethylamine is added to the resin in a ten-fold molar excess, then DMF is added to dissolve it, and the reaction is shaken at room temperature for 30 minutes; then methanol is added to incubate for 20 minutes; the reactive sites on the resin are sealed; Wash the resin repeatedly with DMF and methanol solvent and remove the solvent. The first amino acid is connected to the resin; After fully washing with ethanol, add one drop each of 5% ninhydrin ethanol solution, 0.3% ascorbic acid solution, and 60% phenol solution, and heat to 105°C for 5 minutes at the same time. If the resin color turns dark blue, then It shows that the amino acid has be...
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