Synthesis method for acrylpimaric acid base dithiadiazole derivative
A technology of propylene pimaric acid base and bisthiadiazole, which is applied in organic chemistry and other fields, can solve problems that have not been reported at home and abroad, and achieve the effects of expanding use, increasing added value, and increasing fat solubility
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Embodiment 1
[0037] The preparation of compound a:
[0038]
[0039] Add 0.0025mol propylene pimaric acid into a 150ml three-neck flask equipped with a reflux condenser, a drying tube and a thermometer, slowly add 15ml of thionyl chloride dropwise at room temperature, and heat to reflux for 4 hours after dropping. After the reaction was completed, excess thionyl chloride was distilled off under reduced pressure to obtain propylene pimaric acid chloride.
[0040] Add 0.01mol thiosemicarbazide, 20ml dioxane and 0.01mol benzoic acid into a 150ml two-necked bottle; slowly add 10ml phosphorus oxychloride dropwise while stirring; after adding, raise the temperature to 80°C for 0.5h; then reflux for 4h . After the reaction, pour the reaction liquid into deionized water, adjust the pH to 9, filter, wash with water, and dry to obtain 2-amino-5-phenyl-1,3,4-thiadiazole.
[0041] Add 0.01 mol of 2-amino-5-phenyl-1,3,4-thiadiazole, 20 ml of dioxane, and 2 ml of triethylamine into a 150 ml two-nec...
Embodiment 2
[0043] Preparation of compound b:
[0044]
[0045] Add 0.0025 mol of acrylic pimaric acid and 0.04 mol of phosphorus trichloride into a 150 ml three-neck flask equipped with a reflux condenser, a drying tube and a thermometer, and heat to reflux for 4 hours after dropping. After the reaction, the excessive phosphorus trichloride was distilled off under reduced pressure to obtain propylene pimaric acid chloride.
[0046]Add 0.01mol thiosemicarbazide, 20ml dioxane and 0.01mol m-toluic acid into a 150ml two-necked bottle; slowly add 10ml phosphorus oxychloride dropwise while stirring; after adding, raise the temperature to 80°C for 0.5h; then reflux Under the reaction 4h. After the reaction, pour the reaction solution into deionized water, adjust the pH to 9, filter, wash with water, and dry to obtain 2-amino-5-m-tolyl-1,3,4-thiadiazole.
[0047] Add 0.01 mol of 2-amino-5-m-tolyl-1,3,4-thiadiazole, 20 ml of dioxane, and 2 ml of triethylamine into a 150 ml two-necked bottle....
Embodiment 3
[0049] Preparation of compound c:
[0050]
[0051] Add 0.0025 mol of acrylic pimaric acid, 20 ml of chloroform, and 0.04 mol of phosphorus pentachloride into a 150 ml three-neck flask equipped with a reflux condenser, a drying tube, and a thermometer, heat to reflux for 3 hours after dropping, and stand to filter. After the reaction, the solvent was distilled off under reduced pressure to obtain propylene pimaric acid chloride.
[0052] Add 0.01mol thiosemicarbazide, 20ml dioxane and 0.01mol p-toluic acid into a 150ml two-necked bottle; slowly add 10ml phosphorus oxychloride dropwise while stirring; after adding, raise the temperature to 80°C for 0.5h; then reflux Under the reaction 4h. After the reaction, pour the reaction liquid into deionized water, adjust the pH to 9, filter, wash with water, and dry to obtain 2-amino-5-p-tolyl-1,3,4-thiadiazole.
[0053] Add 0.01 mol of 2-amino-5-p-tolyl-1,3,4-thiadiazole, 20 ml of dioxane, and 2 ml of triethylamine into a 150 ml tw...
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