1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole compound and application thereof
A thiadiazole and triazolo technology is applied in the field of anticancer drugs and achieves the effects of simple process, strong anticancer activity and easy implementation
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Embodiment 1
[0023] 3-Phenyl-6-n-butyldithio-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole, the preparation steps are as follows:
[0024] 1) In a 100ml round-bottomed flask, add 12.21g (80.0mmmol) of methyl benzoate (80.0mmmol) and 30ml (excess) of hydrazine hydrate in sequence, and reflux at 80°C for 5h. After the reaction is complete, cool at low temperature to precipitate a solid, suction filter, and dry to obtain benzene Formic hydrazide.
[0025] 2) Take 6.15g (44.0mmol) of benzohydrazide and 3.12g (53.6mmol) of potassium hydroxide and dissolve them in 50ml of absolute ethanol with stirring at room temperature, drop 3ml (0.005mol) of carbon disulfide at 5°C, and immediately produce a white precipitate. Continue to react for 4 hours, filter with suction, and reflux with hydrazine hydrate (35ml, 85wt%) at 80°C for 6 hours. Recrystallize with absolute ethanol to obtain 3-phenyl-4-amino-5-mercapto-1,2,4-triazole.
[0026] 3) Take 2.03g (0.015mol) of 3-phenyl-4-amino-5-mercapto-1,2,4-triazole...
Embodiment 2
[0030] 3-Phenyl-6-isobutyldithio-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole, the preparation steps are as follows:
[0031] 1) In a 100ml round-bottomed flask, add 12.21g (80.0mmmol) of methyl benzoate (80.0mmmol) and 30ml (excess) of hydrazine hydrate in sequence, and reflux at 80°C for 5h. After the reaction is complete, cool at low temperature to precipitate a solid, suction filter, and dry to obtain benzene Formic hydrazide.
[0032] 2) Take 6.15g (44.0mmol) of benzohydrazide and 3.12g (53.6mmol) of potassium hydroxide and dissolve them in 50ml of absolute ethanol with stirring at room temperature, drop 3ml (0.005mol) of carbon disulfide at 5°C, and immediately produce a white precipitate. Continue to react for 4 hours, filter with suction, and reflux with hydrazine hydrate (35ml, 85wt%) at 80°C for 6 hours. Recrystallize with absolute ethanol to obtain 3-phenyl-4-amino-5-mercapto-1,2,4-triazole.
[0033] 3) Take 2.03g (0.015mol) of 3-phenyl-4-amino-5-mercapto-1,2,4-triazol...
Embodiment 3
[0037] 3-p-methoxyphenyl-6-n-butyldithio-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole, the preparation steps are as follows:
[0038] 1) In a 100ml round bottom flask, add 14.64g (80.0mmmol) of methyl p-methoxybenzoate (80.0mmmol) and 30ml of hydrazine hydrate (excess) and reflux at 80°C for 5h. After the reaction is complete, cool at low temperature to precipitate a solid, filter and dry That is, p-methoxybenzohydrazide.
[0039] 2) Take 8.05g (44.0mmol) of p-methoxybenzoyl hydrazide and 3.12g (53.6mmol) of potassium hydroxide and dissolve them in 50ml of absolute ethanol with stirring at room temperature, add 3ml (0.005mol) of carbon disulfide dropwise at 5°C, immediately Produce white precipitate, continue to react for 4h, filter with suction, and then reflux with hydrazine hydrate (35ml, 85wt%) at 80°C for 6h, pour into 150ml of ice water after the reaction is complete, adjust the pH value to 3-4 with concentrated hydrochloric acid, and generate a large amount of precipitate ,...
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