1,1-Dimethyl-β-carbolinecarboxylic acid modified RGD peptide, its synthesis, antithrombotic effect and application
A carboline carboxylic acid, dimethyl technology, applied in the field of RGD peptide, can solve the problem of no antithrombotic compound
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Embodiment 1
[0062] Embodiment 1 prepares Boc-Ala
[0063]Under ice-bath stirring, 5g (56.18mmol) Ala was dissolved in 160ml of distilled water, and then the pH value was adjusted to 8 with 2N NaOH solution, and 15.92g (73.0mmol) (Boc) was dissolved with 160ml dioxane 2 O is dissolved, then added to the reaction flask, under ice-bath stirring, 2N NaOH solution is added dropwise to adjust the pH to 9, and water or dioxane is added, and the volume ratio of water and dioxane in the reaction solution is 1:1. The pH value of the reaction solution was adjusted to 9, and CO was pumped from time to time. 2 , to promote the reaction to the right, and after 48 hours of reaction, the raw materials disappeared. Reaction compound with saturated KHSO 4 Adjust the pH of the reaction solution to 7, concentrate under reduced pressure to remove dioxane, and then wash the residue with saturated KHSO 4 Adjust the pH of the reaction solution to 2, extract with ethyl acetate, a small amount of multiple times...
Embodiment 2
[0064] Embodiment 2 prepares Tos·Gly-OBzl
[0065] Weigh 7.5g (100mmol) of Gly, add 18.06g (105mmol) of p-toluenesulfonic acid, 60ml of benzyl alcohol and 30ml of cyclohexane, and place the mixture in an oil bath that has been heated to 90°C in advance. Install the water separator and condenser, start the reaction, TLC (dichloromethane:methanol 5:1) after 24h shows that the raw material disappears, the oil bath is lowered to room temperature, add a large amount of ether, stir, and filter after the precipitation is complete to obtain 27.5 g (81%) of the title compound as a colorless solid. Mp132-133℃.ESI-MS(m / e)338[M+H] + .
Embodiment 3
[0066] Embodiment 3 prepares Boc-Ala-Gly-OBzl
[0067] Weigh 3.36g (17.7mmol) Boc-Ala and dissolve it with 80ml of anhydrous THF, add 2.40g (17.7mmol) of HOBt in an ice bath, and add 3.67g (17.7mmol) of DCC and anhydrous THF after 10min The solution, stirred for 30min, is called solution I. 5g (14.8mmol) of Tos·Gly-OBzl was dissolved in anhydrous THF, N-methylmorpholine was added dropwise to adjust the pH to 9, and stirred for 30min, which was called solution II. Mix solution I and solution II, react at room temperature for 8 hours, monitor the disappearance of the reaction raw materials on a TLC board, filter the reaction solution after stopping the reaction, and concentrate the filtrate to dryness under reduced pressure. Add petroleum ether to the viscous substance obtained, continue to grind and wash, and then let it stand and pour, the remaining substance is dissolved with ethyl acetate, and saturated NaHCO 3 Alkaline wash, then saturated KHSO 4 After acid washing and f...
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