Imidazolisopropylacetyltheaninecarbobenzoxypyridoindole, and preparation method, nanostructure and application thereof
A technology of imidazole isopropylacetyl and benzyl theanine, which is applied in the field of biomedicine, can solve problems such as the understanding of value drug designers, and achieve the effect of wide clinical application prospects
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Embodiment 1
[0032] Embodiment 1 prepares 3S-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (1)
[0033] Put 200mL of water in a 250mL round bottom flask, and slowly add 0.1mL of concentrated sulfuric acid. 2.52 g (12.4 mmol) of L-tryptophan was added to the obtained dilute sulfuric acid solution and ultrasonically oscillated until the L-tryptophan was completely dissolved. To the resulting solution was added 5 mL of 37-40% formaldehyde solution. The reaction mixture was stirred at room temperature for 6 hours. The disappearance of L-tryptophan was detected by thin layer chromatography, and the reaction was terminated. Concentrated ammonia water was slowly added dropwise to the reaction solution to adjust the reaction mixture to pH 6, and allowed to stand for 30 minutes. The resulting precipitate filtered out under reduced pressure was repeatedly rinsed with water and acetone three times to obtain 2.64 g (99%) of the title compound as a colorless powder.
[0034] ESI-MS(m / e)215[M-H] ...
Embodiment 2
[0035] Embodiment 2 prepares 3S-N-Boc-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (2)
[0036] Add 20 mL of DMF to a 100 mL eggplant bottle, and add 2.033 g (9.41 mmol) of 3S-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (compound 1) under stirring to obtain a suspension. Add 2.752g (12.6mmol) Boc 2 O, and added triethylamine to adjust the pH of the reaction solution to 10. The reaction mixture was stirred at room temperature for 48 hours, monitored by thin layer chromatography until compound 1 disappeared, the reaction was terminated, and concentrated to dryness under reduced pressure. The resulting oil was dissolved in 100 mL of ethyl acetate and washed with KHSO 4 (5%) aqueous solution (10 mL×3). The combined ethyl acetate layers were separated, dried over anhydrous sodium sulfate for 2 hours, and filtered under reduced pressure. The filtrate was concentrated to dryness under reduced pressure, and a colorless solid was precipitated. The obtained colorless solid...
Embodiment 3
[0037] Example 3 Preparation of 3S-N-Boc-1,2,3,4-tetrahydro-β-carboline-3-formyl-L-leucine benzyl ester (3)
[0038] Add 2.243g (7.10mmol) 3S-N-Boc-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (2) to 250mL eggplant bottle under ice bath, 4.90g (12.4mmol )TosH·Leu-OBzl, 1.402g (10.4mmol) HOBt and 80mL anhydrous THF, stirred to dissolve, 2.589g (12.6mmol) DCC was dissolved in 10mL anhydrous THF, and slowly added dropwise to the reaction flask under ice bath , stir well for 5 minutes. The pH of the reaction mixture was adjusted to 8 with NMM, stirred at 0°C for 4 hours, and DCU was filtered off. The filtrate was concentrated to dryness under reduced pressure. The obtained residue was dissolved in 150 mL of ethyl acetate, placed in a 250 mL separatory funnel, washed successively with saturated aqueous sodium bicarbonate (30 mL×3), saturated aqueous sodium chloride (30 mL×3), 5% potassium bisulfate Wash with aqueous solution (30mL×3), wash with saturated aqueous sodium chlor...
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