Method for preparing collagen sugar
A technology of glycine and chloroacetic acid, applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc., can solve the problems of large solvent consumption and recovery, large solvent loss, large catalyst consumption, etc., and achieve no three-waste pollution. , the solvent loss is small, the effect of saving equipment
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Embodiment 1
[0023] Add 96.5g of 98% chloroacetic acid (1.0moL), 200mL of methanol, 14g of urotropine (0.1moL) into a 500mL four-neck flask equipped with a stirrer, reflux condenser, and thermometer, and start stirring at a speed of about 150r / Min, add 30g of 99.5% ethylenediamine (0.5moL) dropwise. Due to the exothermic reaction, control the reaction temperature to be below 60°C. The dropping speed is from fast to slow. The dropwise addition is completed in 20 minutes, and then heated to 63°C after maintaining for about 15 minutes. Left and right, reduce the stirring speed to about 30r / min, pass through ammonia gas, and then generate a precipitate and turn it into a slurry liquid, check by HPLC, stop the reaction when the peak of monochloroacetic acid disappears, and pass through ammonia gas about 25g , the required time is 2.5 hours, stop stirring and cool down to about 45°C, filter and rinse the filter cake with 20mL of methanol at about 40°C, the filter cake is dried to 98.8%, and the ...
Embodiment 2
[0026] Add 96.5g 98% chloroacetic acid (1.0moL) in the 500mL four-neck flask with stirrer, reflux condenser, thermometer, add dropwise and reclaim the gained filtrate (gained 320mL filtrate after the above-mentioned embodiment 1 sodium chloride is filtered), start Stir at a speed of about 150r / min, keep the reaction temperature below 60°C, drop the speed from fast to slow, finish adding in 20 minutes, keep it for about 15 minutes, then heat to about 63°C, reduce the stirring speed to about 30r / min, Feed ammonia gas, then generate precipitate and become cloudy and become slurry liquid, check by HPLC, stop reaction when the wave peak of monochloroacetic acid disappears, feed ammonia gas about 25g required time 2.5 hours, stop stirring and cool down to At about 45°C, filter and rinse the filter cake with 20mL of methanol at about 40°C, the filter cake is dried to 98.5%, and the product is about 74.2g.
[0027] Add 98g 50% sodium methoxide (about 0.9moL) in 320mL filtrate, fully s...
Embodiment 3
[0029] Add 96.5g of 98% chloroacetic acid (1.0moL), 200mL of ethanol, 14g of urotropine (0.1moL) into a 500mL four-neck flask with a stirrer, reflux condenser, and thermometer, start stirring at a speed of about 150r / min, add 101g of 99.5% triethylamine (1.0moL) dropwise, control the reaction temperature to be below 60°C, the rate of addition changes from fast to slow, and the dropwise addition is completed in 20 minutes, after maintaining for about 15 minutes, heat to about 63°C, and reduce the stirring speed Ammonia gas is injected at about 30r / min, and then a precipitate becomes cloudy and becomes a slurry liquid. Check by HPLC, and stop the reaction when the peak of monochloroacetic acid disappears. It takes 2.5 hours to inject about 25g of ammonia gas, and then stop. Stir and cool down to about 45°C, filter and rinse the filter cake with 20mL of ethanol at about 40°C, dry the filter cake to obtain 98.6%, and the product is about 73.2g.
[0030] Add 168g 50% potassium eth...
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