A kind of bisthiadiazole derivative and preparation method thereof
A technology of bisthiadiazole and derivatives, applied in lubricating compositions, petroleum industry, additives, etc., to achieve the effects of good solubility and excellent extreme pressure
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Embodiment 1
[0038] Add 15.0g of 2,5-dimercapto-1,3,4-thiadiazole (0.1mol) and 80ml of ethyl acetate into a 500ml four-neck flask equipped with a reflux condenser and a thermometer, stir to dissolve, and add 4.0 gNaOH (0.1mol) aqueous solution 20mL, dropwise time is 10min, then add 0.3g tetrabutylammonium bromide (0.001mol) as a catalyst, add 13.7g (0.1mol) bromobutane dropwise at 20 ℃, dropwise The time is 30 minutes. After the dropwise addition, gradually raise the temperature to 76°C for reflux reaction for 4 hours. After the reaction, cool to room temperature and filter to obtain light yellow solid powder 2-thiobutyl-5-mercapto-1,3,4-thiol Oxadiazole.
Embodiment 2
[0040] Add 15.0g 2,5-dimercapto-1,3,4-thiadiazole (0.1mol) and 80ml ethanol in a 500ml four-neck flask equipped with a reflux condenser and a thermometer, stir to dissolve, add dropwise 4.4gNaOH ( 0.11mol) aqueous solution 21mL, dropwise time is 20min, then add 0.3g tetrabutylammonium bromide (0.001mol) as catalyst, drop 14.9g (0.1mol) chlorooctane at 20 ℃, dropwise time is After 40 minutes, after the dropwise addition, gradually raise the temperature to 76°C for reflux reaction for 6 hours. After the reaction, cool to room temperature and filter to obtain light yellow solid powder 2-thiooctyl-5-mercapto-1,3,4-thiadiazole .
Embodiment 3
[0042] Add 20.5g of 2-thiobutyl-5-mercapto-1,3,4-thiadiazole (0.1mol) synthesized in Example 1 in a 500ml four-neck flask equipped with a reflux condenser and a thermometer, and use 75ml of distilled water as a solvent Stir the reaction, add dropwise oxidant 0.12mol hydrogen peroxide (30%) 13.6g, dropwise time is controlled at 10 ~ 15min, then raise the temperature and reflux temperature to react for 6h, after the reaction is finished, extract the product with petroleum ether, pour out the liquid separation, and wash with water until Neutral, after drying with anhydrous sodium sulfate, the solvent is evaporated to obtain a light yellow liquid product bis-5,5'-dithiobis-(1,3,4-thiadiazole-2-thiobutyl) additive . The S content of the product is 45.44%, and the theoretical S content is 46.82%.
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