3-methylpyrido[1,2-a]pyrimidinone derivatives containing 1-((4-substituted benzyl)oxy) and their application
A 2-a, derivative technology, used in applications, biocides, chemicals for biological control, etc., can solve problems such as unreported research on agricultural antibacterial activity
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Embodiment 1
[0058] Example 1: 1-(4-Hydroxy-methoxybenzyl)-3-methyl-2-oxo-1,2-dihydropyrido[1,2-a]pyrimidin-5-ium-4 -Synthetic (compound numbering is A1) of phenate, comprises the following steps:
[0059] (1) Use 2-methylmalonic acid (10mmol), 2,4,6-trichlorophenol (20mmol), and 30 mL of phosphorus oxychloride as solvents, and heat to reflux for 4 to 6 hours. After the reaction is completed, the reaction system Slowly drop into 200mL ice water with magnetic stirring and stir well. After the temperature dropped to room temperature, the white solid was collected by filtration to obtain the intermediate bis(2,4,6-trichlorophenyl)-2-methylmalonate;
[0060] (2) Add 2-aminopyridine (2.0mmol), vanillin (1.5mmol) and DCE 30mL as a solvent into a 100mL three-neck flask for reflux reaction for 3-5h. Add NaBH to the system in batches after the reaction conversion is complete 4 (4.0mmol) as a reducing agent, reflux reaction for 1-2h, after the reaction is completed, remove the solvent under reduc...
Embodiment 2
[0062] Example 2: 1-(4-((2,4-dichlorobenzyl)oxy)-3-methoxybenzyl)-3-methyl-2-oxo-1,2-dihydropyridine The synthesis of [1,2-a] pyrimidine-5-ium-4-phenol salt (the compound number is A2) comprises the following steps:
[0063] (1) with the (1) step of embodiment 1;
[0064] (2) Add vanillin (5.0mmol), potassium carbonate (15.0mmol), 2,3-dichlorobenzyl chloride (6.0mmol), and 30mL of acetonitrile as solvent into a 100mL three-necked flask, and reflux for 3-5h. After the reaction was completed, ice water was added for washing, and then the solid intermediate 4-((2,4-dichlorobenzyl)oxy)-3-methoxybenzaldehyde was collected by filtration;
[0065] (3) 2-aminopyridine (2.0mmol), 4-((2,4-dichlorobenzyl)oxy)-3-methoxybenzaldehyde (1.5mmol), with DCE 30mL as solvent, was added to Reflux reaction in a 100mL three-neck flask for 3-5 hours. After the reaction is converted, add NaBH to the system in batches 4 (4.0mmol) as a reducing agent, reflux reaction for 1-2h, after the reaction is ...
Embodiment 3
[0067]Example 3: 1-(4-((3-chlorobenzyl)oxy)-3-methoxybenzyl)-3-methyl-2-oxo-1,2-dihydropyrido[1 , 2-a] the synthetic (compound number is A3) of pyrimidin-5-ium-4-phenol salt, comprises the following steps:
[0068] (1) with the (1) step of embodiment 1;
[0069] (2) Add vanillin (5.0mmol), potassium carbonate (15.0mmol), 3-chlorobenzyl chloride (6.0mmol), and 30mL of acetonitrile as a solvent into a 100mL three-necked flask, and reflux for 3-5h. After the reaction is completed, Add ice water to wash, then collect the solid intermediate 4-((3-chlorobenzyl)oxy)-3-methoxybenzaldehyde by filtration;
[0070] (3) Add 2-aminopyridine (2.0mmol), 4-((3-chlorobenzyl)oxy)-3-methoxybenzaldehyde (2.0mmol) to a 100mL three-necked flask with DCE 30mL as solvent Medium reflux reaction for 3 to 5 hours. After the reaction is converted, add NaBH to the system in batches 4 (4.0mmol) as a reducing agent, reflux reaction for 1-2 h, after the reaction was completed, the solvent was removed und...
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