Beta-amino ethyl thiosulfuric acid and synthesis method thereof
A technology of aminoethyl thiosulfuric acid and feed additives, applied in animal feed, animal feed, organic chemistry, etc., can solve problems such as obesity and affecting meat quality, and achieve increased reaction temperature, improved safety, and product yield high effect
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Embodiment 1
[0027] The synthetic method 1 of β-aminoethylthiosulfuric acid, concrete steps are:
[0028] 1) Preparation of ethyl chloride hydrochloride:
[0029] Add 150g of ethanolamine hydrochloride to the reaction vessel, then add 300g of anhydrous chlorobenzene, stir evenly, keep the temperature at 80°C, add 450g of thionyl chloride dropwise at a rate of 1.5g / min, and continue stirring for 1 hour after dropping , then cooled to 30°C, added 210 ml of water, 7.5 g of activated carbon, stirred for 0.5 h, discharged and filtered, and the filtrate was allowed to stand for stratification.
[0030] 2) Preparation of β-aminoethylthiosulfuric acid
[0031] Take the lower layer of ethyl chloride hydrochloride solution, 45 ~ 55 ℃ rotary evaporation under reduced pressure until anhydrous, to obtain a viscous liquid, control the temperature at 70 ℃, add 600g of sodium thiosulfate, keep stirring for 2 hours and then quickly filter while hot , the filtrate was cooled to 10°C, crystallized, filtere...
Embodiment 2
[0033] The synthetic method 2 of β-aminoethyl thiosulfuric acid, concrete steps are:
[0034] 1) Preparation of ethyl chloride hydrochloride:
[0035] In reaction vessel, add 160g ethanolamine hydrochloride, then add 320 g Anhydrous chlorobenzene, stir evenly, keep the temperature at 80°C, add 480g of thionyl chloride dropwise at a rate of 1.5g / min, continue stirring for 1 hour after dropping, then cool to 30°C, add 220ml of water, 8.0g Activated carbon, after stirring for 0.5h, discharge and filter, and the filtrate is allowed to stand for stratification.
[0036] 2) Preparation of β-aminoethylthiosulfuric acid
[0037] Take the lower layer of ethyl chloride hydrochloride solution, 45 ~ 55 ℃ rotary evaporation under reduced pressure until anhydrous, to obtain a viscous liquid, control the temperature at 70 ℃, add 640g of sodium thiosulfate, keep stirring for 2 hours, then quickly filter while hot , the filtrate was cooled to 10°C, crystallized, filtered, and the solid was ...
Embodiment 3
[0039] The synthetic method 3 of β-aminoethylthiosulfuric acid, concrete steps are:
[0040] 1) Preparation of ethyl chloride hydrochloride:
[0041] Add 170g ethanolamine hydrochloride in reaction vessel, add 340 g Anhydrous chlorobenzene, stir evenly, keep the temperature at 80°C, add 510g of thionyl chloride dropwise at a rate of 1.5g / min, continue stirring for 1 hour after dropping, then cool to 30°C, add 230ml of water, 8.5g Activated carbon, after stirring for 0.5h, discharge and filter, and the filtrate is allowed to stand for stratification.
[0042] 2) Preparation of β-aminoethylthiosulfuric acid
[0043] Take the lower layer of ethyl chloride hydrochloride solution, 45 ~ 55 ℃ rotary evaporation under reduced pressure until anhydrous, to obtain a viscous liquid, control the temperature at 70 ℃, add 680g of sodium thiosulfate, keep stirring for 2 hours and then quickly filter while hot , the filtrate was cooled to 10°C, crystallized, filtered, and the solid was drie...
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