N-substituted phenyl-2-((1H-benzimidazole-2-group) sulfydryl) amides derivatives and usage thereof
A technology of benzimidazole and acetamide, applied in the field of organic compound synthesis and pharmaceutical application, to achieve obvious anti-HIV-1 virus activity, high selectivity index, and small cytotoxic effect
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Embodiment 1
[0028] Example 1: Intermediate 2-((1 H -Benzimidazol-2-yl)-mercapto)- N -(2-trifluoromethyl) phenyl) acetamide synthesis, concrete operations are as follows:
[0029]
[0030] Add 2-mercapto-1 to a dry three-necked flask H -Benzimidazole (0.02mol), dissolved in 10ml DMF, added anhydrous potassium carbonate solid (0.02mol), gradually heated to 70°C, added 2-bromo- N -(2-(trifluoromethyl)phenyl)acetamide, continue stirring reaction at 70°C, TLC tracking for about 4 hours, reactant 2-bromo- N -(2-(Trifluoromethyl)phenyl)acetamide disappeared. The reaction was stopped, and the reaction solution was poured into ice water to precipitate a precipitate, which was filtered under reduced pressure and dried to obtain a crude product, which could be directly used in the next step without purification.
Embodiment 2
[0031] Example 2 : N -(3-Bromophenyl)-2-((1-cyclohexylcarbonyl)-1 H - the synthesis of benzo [d] imidazol-2-yl) mercapto) acetamide (Ia), the specific operations are as follows:
[0032] Add 2-((1 H -Benzimidazol-2-yl)-mercapto)- N -(3-Bromophenyl)acetamide (0.002mol), dissolved in 5ml of DMF and then added to 0.5ml of triethylamine solution to adjust the pH value to 8. Cyclohexylformyl chloride liquid (0.002mol) was added, and the temperature was gradually raised to 65°C. After TLC followed the reaction for 6 hours, the reactant cyclohexylformyl chloride disappeared. The reaction was stopped, and the reaction solution was poured into ice water to precipitate a precipitate, which was filtered, washed three times with absolute ethanol, and dried by suction to obtain a crude product. After the crude product was subjected to column chromatography (petroleum ether: ethyl acetate = 3:1), a pure white solid Ia was obtained. The test results are as follows:
[0033] the I...
Embodiment 3
[0035] Example 3 : N -(3,5-difluorophenyl)-2-((1-cyclohexylcarbonyl)-1 H - Benzo [d] imidazol-2-yl) mercapto) acetamide (Ib) synthesis, concrete operations are as follows:
[0036] Add 2-((1 H -Benzimidazol-2-yl)-mercapto)- N -(3,5-difluorophenyl)acetamide (0.002mol), dissolved in 5ml of DMF, then added 0.5ml of triethylamine solution, and adjusted the pH value to 8. Cyclohexylformyl chloride liquid (0.002mol) was added, and the temperature was gradually raised to 65°C. After TLC followed the reaction for 6 hours, the reactant cyclohexylformyl chloride disappeared. Stop the reaction, pour the reaction solution into ice water, precipitate the precipitate, filter, wash the product with absolute ethanol 3 times, filter and dry to obtain the crude product. After the crude product is subjected to column chromatography (petroleum ether: ethyl acetate=3:1), a white solid Ib is obtained, and the detection results are as follows:
[0037] Ib
[0038] Yield: 17.4%; Melting p...
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