Method for preparing betaine hydrochloride
A technology of betaine hydrochloride and hydrochloric acid, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, can solve the problems of high energy consumption, large alcohol solvent consumption, cumbersome operation, etc., and achieve high yield, The effect of less raw material consumption and simple separation
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Embodiment 1
[0015] Add 394g of trimethylamine aqueous solution with a mass fraction of 33% into the reaction flask, cool down to about 0°C, add 94.5g of chloroacetic acid in batches under stirring, seal the reaction device, stir at 20-30°C for 1 hour, then heat up to 50°C React at ~60°C for 1.5h, then raise the temperature to 80-90°C for 0.5h. After the reaction is over, use 37% hydrochloric acid to adjust the pH to 1 to 3, raise the temperature, evaporate the water in the solution under reduced pressure, add an appropriate amount of chloroform, reflux for 15 minutes, heat filter, and filter the cake with a small amount of After washing with chloroform, dry and weigh to obtain betaine hydrochloride 147.34g, the yield in terms of chloroacetic acid is 96.2%, and the purity is 99.2%; the filtrate evaporates the solvent, and the gained solid is the hydrochloride of trimethylamine, weighing 108g , 99.5%.
Embodiment 2
[0017] Add 325g of trimethylamine aqueous solution with a mass fraction of 40% in the reaction flask, cool down to about 0°C, add 94.5g of chloroacetic acid in batches under stirring, seal the reaction device, stir at 20-30°C for 1 hour, then heat up to 50°C React at ~60°C for 1.5h, then raise the temperature to 80-90°C for 0.5h. After the reaction is over, use 20% hydrochloric acid to adjust the pH to 1 to 3, raise the temperature, evaporate the water in the solution under reduced pressure, add an appropriate amount of ethanol, reflux for 15 minutes, heat filter, and filter the cake with a small amount of ethanol After washing, dry and weigh to obtain betaine hydrochloride 146.5g, the yield in terms of chloroacetic acid is 95.7%, and the purity is 99.3%; 99.6%.
Embodiment 3
[0019] Add 325g of trimethylamine aqueous solution with a mass fraction of 40% in the reaction flask, cool down to about 0°C, add 94.5g of chloroacetic acid in batches under stirring, seal the reaction device, stir at 20-30°C for 1 hour, then heat up to 50°C React at ~60°C for 1.5h, then raise the temperature to 80-90°C for 0.5h. After the reaction is over, adjust the pH to 1.5 with 37% hydrochloric acid, increase the temperature, evaporate the water in the solution under reduced pressure, add an appropriate amount of ethanol, reflux for 15 minutes, heat filter, and filter the cake with a small amount of chloroform After washing with the mixed solution of ethanol (volume ratio is 1: 1), dry and weigh to obtain betaine hydrochloride 148.2g, in terms of chloroacetic acid, the yield is 96.8%, and the purity is 99.5%; the filtrate evaporates the solvent, and the gained solid is trimethylamine The hydrochloride, weighing 108.1g, purity is 99.7%.
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