Chalcone derivative containing thioether triazole, preparation method and application
A kind of derivative, the technology of chalcone is applied in the field of preparation of chalcone derivatives to achieve excellent effect of inhibiting plant pathogens
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Embodiment 1
[0028] 1-(4-(2-((4-Amino-5-methyl-4H-1,2,4-triazol-3-yl)thio)ethoxy)phenyl)-3-(thiophene- 2-yl)-2-propen-1-one (target compound B 1 ) preparation method, comprising the following steps:
[0029] (1) Preparation of hydrazinothiohydrazide (intermediate 1):
[0030] Add 20mL of 85% hydrazine hydrate and 60mL of water to a three-neck flask equipped with a thermometer, dropping funnel and condenser (the upper port is connected with a tail gas outlet pipe), and control the temperature at about 50°C. Under electromagnetic stirring, 6 mL of CS2 was added dropwise within 1 h, and then the mixed solution was refluxed at 90° C. for 1 h, cooled and crystallized, filtered with suction, and recrystallized in water to obtain colorless needle-shaped crystals (intermediate 1), yield: 82% .
[0031] (2) Preparation of 4-amino-5-methyl-4H-1,2,4-triazole-3-mercapto (intermediate 2):
[0032] Take 3.18g (0.03mol) of hydrazinothiohydrazide (intermediate 1) in a flask, add 10mL of glacial acetic...
Embodiment 2
[0040] 1-(2-(2-((4-Amino-5-methyl-4H-1,2,4-triazol-3-yl)thio)ethoxy)phenyl)-3-(thiophene- 2-yl)-2-propen-1-one (target compound B 2 ) preparation method, comprising the following steps:
[0041] (1) Preparation of hydrazinothiohydrazide (intermediate 1):
[0042] As in the first (1) step of Example 1.
[0043] (2) Preparation of 4-amino-5-methyl-4H-1,2,4-triazole-3-mercapto (intermediate 2):
[0044] As in embodiment 1 (2) step.
[0045] (3) Preparation of 1-(2-hydroxyphenyl)-3-(thiophen-2-yl)-2-propen-1-one (intermediate 3):
[0046] As in step (3) of Example 1, the difference is that X is 2-O.
[0047] (4) Preparation of 1-(thiophen-2-yl)-3-(4-(2-bromoethoxy)phenyl)-chalcone (intermediate 4):
[0048] As in step (4) of Example 1, the difference is that X is 2-O.
[0049] (5) 1-(2-(2-((4-amino-5-methyl-4H-1,2,4-triazol-3-yl)thio)ethoxy)phenyl)-3- (Thien-2-yl)-2-propen-1-one (target compound B 2 ) preparation:
[0050] As in step (5) of Example 1, the difference is t...
Embodiment 3
[0052] 1-(2-(2-((4-Amino-5-methyl-4H-1,2,4-triazol-3-yl)thio)ethoxy)phenyl)-3-(4- Nitro)-2-propen-1-one (target compound B 3 ) preparation method, comprising the following steps:
[0053] (1) Preparation of hydrazinothiohydrazide (intermediate 1):
[0054] As in the first (1) step of Example 1.
[0055] (2) Preparation of 4-amino-5-methyl-4H-1,2,4-triazole-3-mercapto (intermediate 2):
[0056] As in embodiment 1 (2) step.
[0057] (3) Preparation of 1-(2-hydroxyphenyl)-3-(4-nitro)-2-propen-1-one (intermediate 3):
[0058] As in step (3) of Example 1, the difference is that X is 2-O, and R is 4-nitrobenzaldehyde.
[0059] (4) Preparation of 1-(4-nitro)-3-(4-(2-bromoethoxy)phenyl)-chalcone (intermediate 4):
[0060] As in step (4) of Example 1, the difference is that X is 2-O, and R is 4-nitrobenzaldehyde.
[0061] (5) 1-(2-(2-((4-amino-5-methyl-4H-1,2,4-triazol-3-yl)thio)ethoxy)phenyl)-3- (4-nitro)-2-propen-1-one (target compound B 3 ) preparation:
[0062] As in step...
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