Method for preparing betaine hydrochloride
A technology of betaine hydrochloride and dilute hydrochloric acid, applied in chemical instruments and methods, cyanide reaction preparation, preparation of organic compounds, etc., can solve the problems of easy existence of safety, high cost, strong irritation, etc., and achieve mild reaction conditions. , safety assurance, cost reduction effect
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Embodiment 1
[0030] A method for preparing betaine hydrochloride, the steps are:
[0031] a. Add 1mol ethyl chloroacetate 122.5g and ethanol 500g in the 1500ml three-neck bottle that reflux condenser, thermometer, air guide tube, tail gas absorption device and magnetic stirring device are housed, be placed on the ice-water bath under stirring, make reaction mixture cool down to Below 10°C;
[0032] b. Pass 59 g of 1 mol of anhydrous trimethylamine gas into the mixture, keep the reaction temperature not exceeding 20°C during the gas flow, continue to stir for 1 hour after passing through, collect the solid product by filtration, and recrystallize through acetonitrile at 90°C / 10mmHg Drying at low temperature for 6 hours gave 173.7 g of 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride, melting point 151-153°C, yield 95.7%;
[0033] c. In a 2000ml three-necked flask equipped with a reflux condenser, a thermometer and a magnetic stirring device, add 181.5g of 1mol of 2-ethoxy-2-oxa-N,N...
Embodiment 2
[0037] A method for preparing betaine hydrochloride, the steps are:
[0038] a. Add 1mol ethyl chloroacetate 122.5g and ethanol 980g in the 1500ml three-neck flask that reflux condenser, thermometer, air guide tube, tail gas absorbing device and magnetic stirring device are housed, be placed on ice-water bath under stirring, make reaction mixture cool down to Below 10°C;
[0039] b. Pass 65g of 1.1mol anhydrous trimethylamine gas into the mixture, keep the reaction temperature not exceeding 20°C during the gas pass-in process, continue to stir for 2 hours after the pass-in is complete, filter and collect the solid product, and recrystallize through acetonitrile at 90°C / Dry at 10 mmHg for 6 hours to obtain 175.5 g of 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride with a melting point of 151-153°C and a yield of 96.7%;
[0040]c. In a 2000ml three-necked flask equipped with a reflux condenser, a thermometer and a magnetic stirring device, add 181.5g of 1mol of 2-etho...
Embodiment 3
[0044] A method for preparing betaine hydrochloride, the steps are:
[0045] a. Add 1mol ethyl chloroacetate 122.5g and isopropanol 370g in the 1500ml three-necked bottle that is equipped with reflux condenser, thermometer, air guide tube, tail gas absorbing device and magnetic stirring device, place on ice-water bath under stirring, make reaction mixture Cool down to below 10°C;
[0046] b. Pass 65g of 1.1mol anhydrous trimethylamine gas into the mixture, keep the reaction temperature not exceeding 20°C during the gas pass-in process, continue to stir for 2 hours after the pass-in is complete, filter and collect the solid product, and recrystallize through acetonitrile at 90°C / Dry at 10mmHg for 6 hours to obtain 162.3g of 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride with a melting point of 151-153°C and a yield of 89.4%;
[0047] c. In a 2000ml three-necked flask equipped with a reflux condenser, a thermometer and a magnetic stirring device, add 181.5g of 1mol o...
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