(3R,12aS)-3-(4-aminobutyl)-2,3,6,7,12,12a-hexahydropyrazino[1',2':1,6]pyrido[3,4-b]indole-1,4-dione, and preparation and application thereof
A 3-b, diketone technology, applied in the field of biomedicine, can solve problems such as no effect
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Embodiment 1
[0023] Embodiment 1 prepares 3S-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (1)
[0024] Add 0.4 mL of concentrated sulfuric acid into 800 mL of distilled water, stir evenly, add 10 g of L-Trp, and sonicate to aid dissolution; add 20 mL of formaldehyde solution to the reaction solution, and stir at room temperature for 10 hours. Post-processing: add concentrated ammonia water dropwise to the reaction solution to adjust the pH to 6, let it stand still, a colorless solid precipitates, filter and dry to obtain 11.32 g of the crude product. ESI-MS (m / e): 215 [M-H] - .
Embodiment 2
[0025] Example 2 Preparation of 3S-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid methyl ester (2)
[0026] Add 60mL of methanol to a 250mL reaction flask, add 7mL of thionyl chloride dropwise under ice bath, activate for 30 minutes, add 6.2g of 3S-1,2,3,4-tetrahydro-β-carboline-3- Carboxylic acid (1), stirred at room temperature overnight, TLC showed that the starting material basically disappeared. Post-processing: remove the solvent under reduced pressure, dissolve the residue with 100 mL of ethyl acetate, adjust the pH to 8 with triethylamine, and purify by silica gel column chromatography (CH 2 Cl 2 :CH 3 OH=100:1-20:1), yielding 4.625 g (70%) of methyl 3S-1,2,3,4-tetrahydro-β-carboline-3-carboxylate as a colorless solid. ESI-MS(m / e): 231[M+H] + .
Embodiment 3
[0027] Example 3 Preparation of 3S-1,2,3,4-tetrahydro-β-carboline-2-(D-Boc-benzyloxycarbonyllysyl)-3-carboxylic acid methyl ester (3)
[0028]Suspend 1.9g (5.0mmol) D-Boc-Lys(Z) in 20mL of anhydrous tetrahydrofuran, add 0.675g (5.0mmol) HOBt to the solution with stirring at room temperature, add 1.133g (5.5mmol) DCC while stirring in an ice bath , to obtain reaction solution I, stirred under ice bath for 30 minutes; 1.15g (5.0mmol) 3S-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid methyl ester (2) was suspended in In 20 mL of anhydrous tetrahydrofuran, the reaction solution II was obtained; the reaction solution II was added to the reaction solution I, stirred for 1 h under ice bath, and stirred overnight at room temperature. Post-treatment: remove DCU by filtration under reduced pressure, concentrate the filtrate under reduced pressure to remove tetrahydrofuran, dissolve the residue with 150mL ethyl acetate, put the obtained solution in a 250mL separatory funnel, and succes...
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