Synthesis, activity and application of dopa-peptide
A compound, -gly-asp technology, applied in the field of biomedicine, can solve problems such as no effective drugs
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Embodiment 1
[0020] Embodiment 1 prepares (S)-3,4-dihydroxyl-Phe-OBzl
[0021] Stir a solution of 1g (5.08mmol) (S)-3,4-dihydroxy-Phe, 1.02g p-toluenesulfonic acid, 8mL benzyl alcohol and 8mL n-hexane at 90-95°C for 36h, cool to room temperature, pour a large amount of diethyl ether A large amount of colorless solid was precipitated, allowed to stand, and filtered. The filter cake was triturated with ether and dried to give 1.08 g (77%) of the title compound as a yellow powder. ESI-MS(m / z): 288[M+H] + .
Embodiment 2
[0022] Embodiment 2 prepares (S)-3,4-dihydroxyl-Phe(Boc-Ala)-OBzl
[0023] Dissolve 207mg (1.1mmol) Boc-Ala in 15mL of anhydrous tetrahydrofuran (THF), add 149mg (1.1mmol) N-hydroxybenzotriazole (HOBt) and 268mg (1.3mmol) dicyclohexylcarbonyldi The anhydrous THF solution of imine (DCC) was stirred in an ice bath for 20 minutes to obtain the corresponding active ester solution. Dissolve 460mg (1.0mmol) of (S)-3,4-dihydroxy-Phe-OBzl in anhydrous THF, then mix with the newly obtained active ester solution, and add N-methylmorpholine (NMM) dropwise to adjust the pH 8. The resulting reaction mixture was reacted at room temperature for 24 hours. Filtration, the filtrate was concentrated to dryness under reduced pressure, the residue was dissolved in ethyl acetate, and the solution was successively washed with saturated KHSO 4 solution was washed 3 times, saturated NaCl solution was washed 3 times, and the obtained ethyl acetate layer was washed with anhydrous NaCl 2 SO 4 Dry, fi...
Embodiment 3
[0024] Embodiment 3 prepares (S)-3,4-dihydroxyl-Phe(Boc-Ala)
[0025] To 458 mg (1.0 mmol) of (S)-3,4-dihydroxy-Phe(Boc-Ala)-OBzl was added 20 mL of methanol and 30 mg of Pd / C. Pass hydrogen into the obtained suspension, stir at room temperature for 24 hours, TLC (CH 2 Cl 2 / MeOH, 30 / 1) to monitor the disappearance of the reaction raw material point. Pd / C was filtered off, and the filtrate was concentrated under reduced pressure to remove the solvent to obtain 319 mg (86%) of the title compound as a colorless powder. ESI-MS(m / z): 367[M-H] - .
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