Dinitrosalicylic xanthate ester compound with hexamethylbenzene structure and preparation method and application thereof
A technology of compound and xanthate, which can be used in medical preparations containing active ingredients, organic chemistry, drug combination, etc., can solve the problems of many toxic and side effects
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Embodiment 1
[0017] The synthesis of embodiment 1 compound I
[0018]
[0019] A. Synthesis of Compound IV-1
[0020] Compound II (1.48 g, 10 mmol) and compound III-1 (2.01 g, 10 mmol) were dissolved in 20 mL of dry CH 2 Cl 2 , stirred at room temperature, added anhydrous AlCl 3 (1.33 g, 10 mmol), then the reaction mixture was stirred overnight at room temperature, TLC showed the reaction was complete. The reaction mixture was poured into 200 mL of ice water, stirred, and washed with CH 2 Cl 2 (60mL×3) for extraction, combined the extract phases, washed with 1% dilute hydrochloric acid and brine successively, and dried over anhydrous sodium sulfate. The desiccant was removed by suction filtration, the filtrate was evaporated to dryness on a rotary evaporator, and the obtained residue was purified by column chromatography to obtain compound IV-1 as a white solid. ESI-MS, m / z=314 ([M+H] + ).
[0021] B. Synthesis of Compound V-1
[0022] Compound IV-1 (1.88g, 6mmol) was dissolve...
Embodiment 2
[0027] The synthesis of embodiment 2 reference compound D-1
[0028] In order to further illustrate the good effect of the compound of the present invention, the application records the compound D-1, which is also invented by the applicant and has not yet been published, and its structure is as follows:
[0029]
[0030] The synthesis method is as follows:
[0031]
[0032] A. Synthesis of Compound IV-2
[0033] Compound II (1.48 g, 10 mmol) and compound III-2 (1.57 g, 10 mmol) were dissolved in 20 mL of dry CH 2 Cl 2 , stirred at room temperature, added anhydrous AlCl 3 (1.33 g, 10 mmol), then the reaction mixture was stirred overnight at room temperature, TLC showed the reaction was complete. The reaction mixture was poured into 200 mL of ice water, stirred, and washed with CH 2 Cl 2 (60mL×3) for extraction, combined the extract phases, washed with 1% dilute hydrochloric acid and brine successively, and dried over anhydrous sodium sulfate. The desiccant was re...
Embodiment 3
[0040] Activation of Example 3 compound to AMPK in vitro
[0041] Human recombinant AMPK enzyme was expressed in E. coli and reactivated in vitro with LKB1 prior to enzyme activity assays. AMPK enzyme activity was detected using two fluorescence-based techniques (α-screen and Delfia) and prepared in microplates (containing 25 mM Tris / HCl buffer, pH 7.5, Hepes buffer containing 100 μM ATP / 50 mM, 25 mM Tris / HCl buffer, pH 7.4, containing 125 μM ATP) in the presence of a synthetic peptide substrate (AMARAASAAALARRR, ie "AMARAA" peptide) and serial dilutions of activator. The reaction was initiated by adding AMPK (50-100 ng). After mixing, the plate was incubated at room temperature for 30 minutes. Enzyme activity was detected by using an antibody against phosphorylated serine to measure the amount of phosphate incorporated into AMARAA. The activity is expressed as a percentage (%) of the control (basal activity is expressed as 100).
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