9-position substituted pyrido[3,4-b]indole derivatives, preparation method thereof and use as sirt protein inhibitor
A technology of substituents and compounds, applied in the field of SIRT protein inhibitors, can solve the problems of no reports of SIRT5 inhibitor drugs
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Embodiment 1
[0107] The preparation of embodiment 1 compound key intermediate of the present invention
[0108] 1. Synthesis of compound 2-(9H-pyrido[3,4-b]indol-9-yl)ethyl acetate (3)
[0109]
[0110] Put the raw material compound 1 (0.50g, 2.98mmol) and NaH (0.24g, 5.96mmol) purchased from Bailingwei CAS No. 244-63-3; Product No. 230515 into a round bottom flask, and then dissolve it with 10mL DMF , after stirring at room temperature for 2 h, compound 2 (0.49 mL, 4.46 mmol) was added dropwise to the above reaction solution, and reacted at room temperature for 5 h, and TLC detected that the reaction of the raw materials was basically complete.
[0111] Add water, extract 3 times with ethyl acetate, the organic layer is dried over magnesium sulfate, after concentrating, the crude product is subjected to silica gel column chromatography (CH 2 Cl 2 :CH 3 OH=60: 1) purification to obtain light yellow solid compound 3 (0.40 g, yield 54%).
[0112] Compound 3: 1 H NMR (400MHz, DMSO-d6)...
Embodiment 2
[0128] The solvent was distilled off under reduced pressure, and saturated NaHCO 3 The pH was adjusted to 8, extracted three times with ethyl acetate, and the organic layer was dried over magnesium sulfate and concentrated to obtain light yellow solid compound 9 (0.12 g, yield 86%). Synthesis of Example 2 Compound N-benzyl-2-(9H-pyrido[3,4-b]indol-9-yl)acetamide (5a)
[0129]
[0130] First use 2mLCH 2 Cl 2 Compound 4 (0.05g, 0.22mmol) was dissolved, and benzylamine (0.05mL, 0.44mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide salt was gradually added under stirring at 0°C salt (EDCI, 0.05g, 0.27mmol), 1-hydroxybenzotriazole (HOBT, 0.04g, 0.27mmol) and N, N-diisopropylethylamine (DIEA, 0.09mL, 0.44mmol), After the addition was completed, the temperature was raised to room temperature and the reaction was stirred for 12 hours. TLC detection showed that the reaction was complete.
[0131] Water was added, extracted three times with dichloromethane, the organic layer w...
Embodiment 3
[0133] Synthesis of Example 3 Compound N-(pyridine-3-methylene)-2-(9H-pyrido[3,4-b]indol-9-yl)acetamide (5b)
[0134]
[0135] First use 2mLCH 2 Cl 2 Dissolve compound 4 (0.03g, 0.13mmol), and gradually add pyridine-3-methylamine (0.03g, 0.26mmol), 1-(3-dimethylaminopropyl)-3-ethyl carbon under stirring at 0°C Diimine hydrochloride (EDCI, 0.03g, 0.16mmol), 1-hydroxybenzotriazole (HOBT, 0.02g, 0.16mmol) and N, N-diisopropylethylamine (DIEA, 0.06mL, 0.26mmol), the addition was completed, the temperature was raised to room temperature, and the reaction was stirred for 12h, and TLC detected that the reaction was complete.
[0136] Water was added, extracted three times with dichloromethane, the organic layer was dried over magnesium sulfate, concentrated, and the crude product was subjected to silica gel column chromatography (CH 2 Cl 2 :CH 3 OH=10:1) was purified to obtain white solid compound 5b (0.03 g, yield 71%).
[0137] Compound 5b: purity: HPLC test is 98%; 1 H N...
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