5-Hydroxytryptophan methyl ester derivative with anti-tumor activity and its preparation method and application
A technology for hydroxytryptophan methyl ester and antitumor activity, which is applied in the field of 5-hydroxytryptophan methyl ester derivatives and their preparation, and can solve the problems of unsatisfactory therapeutic effect, enhanced systemic toxic and side effects, and reduced effective drug concentration.
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[0017] Synthesis of 5-hydroxy-N-[[1-(4-tert-butylbenzyl)-1H-1,2,3-triazol-4-yl]carbonyl]-D-tryptophan methyl ester :
[0018]
[0019] a: NaN 3 , DMF, rt, 12h; b: CuSO 4 , Sodium ascobate, THF-H 2 O(1:1), rt, 5h; c: LiOH, THF-MeOH-H 2 O(4:2:1), rt, over night; d: SOCl 2 , MeOH, reflux, 5h; e: EDC·HCl, HOBt, DMF, triethylamine, rt, over night.
[0020] The specific steps of the synthesis process are:
[0021] 1) Synthesis of 5-hydroxytryptophan methyl ester
[0022] Add 44.00 g (0.2 mol) of 5-hydroxytryptophan and 350 mL of methanol into a 500 mL three-necked flask, cool down to -5°C, and slowly add 17.4 mL (0.24 mol) of thionyl chloride dropwise at low temperature. After the dropwise addition, the temperature was raised to 35° C. to react overnight. TLC detects that the raw material disappears and stops the reaction. Methanol was distilled off under reduced pressure, and after cooling, 300 mL of ethyl acetate was added to stir, filtered with suction, and dried to o...
experiment example 1
[0032] The purpose of this test example is to study the in vitro anti-tumor cell proliferation activity of the compound of the present invention
[0033] Human esophageal squamous cell carcinoma cells (TE-1), human gastric carcinoma cells (MGC803), and human colon carcinoma cells (HCT116) in the logarithmic growth phase were divided into 6×10 3 Each well was inoculated into a 96-well plate, and after 24 hours of culture, the medium was replaced with 5-hydroxy-N-[[1-(4-tert-butylbenzyl)-1H-1,2,3-triazol Azol-4-yl]carbonyl]-D-tryptophan methyl ester medium, 9 concentrations for each sample, respectively 128, 64, 32, 16, 8, 4, 2, 1, 0.5 μg / mL, A blank control group was set up, and culture continued for 72 hours. After the culture is over, add 20 μL of MTT to each well, discard the medium after four hours, add 150 mL of DMSO to each well, measure the OD value with a microplate reader at a wavelength of 490 nm after shaking evenly, and calculate the IC of the compound using SPSS s...
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