Benzimidazole amide bactericide
A technology of benzimidazolone amide and agricultural fungicide, applied in the field of pesticides, can solve problems such as unreported bacteriostatic activity, and achieve the effects of high reaction yield and product purity, simple raw materials, and few synthesis steps
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Embodiment 1
[0028] 1. Synthesis of 1-(prop-1-en-2-yl)-3-propionyl-1H-benzimidazol-2-one
[0029] In the reaction flask equipped with a water separator, add 54g (0.5mol) o-phenylenediamine and 220mL xylene, after heating and stirring to reflux, slowly add 71.5g (0.55mol) of ethyl acetoacetate and mix with 20mL xylene After dripping, stir and reflux for azeotropic dehydration until no water drops appear, then continue to stir and reflux for 2 hours. After completion of the reaction, cool down to precipitate crystals, filter and dry to obtain 76.5 g of white granular crystals (yield 87.9%), which is the intermediate 1-isopropenyl-1,3-dihydro-2H-benzimidazole-2- Ketone, melting point 120~122℃. Take 1.74g (0.01mol) of the intermediate 1-isopropenyl-1,3-dihydro-2H-benzimidazol-2-one and 0.01mol of triethylamine dissolved in 30mL of toluene, add dropwise at room temperature 0.01mol of propionyl chloride solution (0.92g of acryloyl chloride dissolved in 10mL of toluene), stirred at room tempera...
Embodiment 2
[0032] 2. Synthesis of 1-acryloyl-3-(prop-1-en-2-yl)-1H-benzimidazol-2-one
[0033] The synthesis of the intermediate 1-isopropenyl-1,3-dihydro-2H-benzimidazol-2-one is the same as in Example 1. Take 1.74g (0.01mol) of intermediate 1-isopropenyl-1,3-dihydro-2H-benzimidazol-2-one and 0.01mol of triethylamine dissolved in 30mL of toluene, add dropwise at room temperature 0.01mol of acryloyl chloride solution (0.90g of acryloyl chloride dissolved in 10mL of toluene), stirred at room temperature for 5-8 hours, washed three times with water, dried and precipitated to obtain 2.11g of the target compound (92.5% yield), melting point 108-110°C .
[0034]
Embodiment 3
[0036] 3. Synthesis of 1-(3-chloropropionyl-3-(prop-1-en-2-yl)-1H-benzimidazol-2-one
[0037] The synthesis of the intermediate 1-isopropenyl-1,3-dihydro-2H-benzimidazol-2-one is the same as in Example 1. Take 1.74g (0.01mol) of intermediate 1-isopropenyl-1,3-dihydro-2H-benzimidazol-2-one and 0.01mol of triethylamine dissolved in 30mL of toluene, add dropwise at room temperature 0.01mol 3-chloropropionyl chloride solution (1.26g 3-chloropropionyl chloride dissolved in 10mL toluene), stirred at room temperature for 5-8h, washed three times with water, dried and precipitated to obtain 2.23g of the target compound (84.4% yield) , Melting point 110~112℃.
[0038]
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