L-alpha-glycerophosphorylcholine impurity and synthesis method thereof
A technology of glycerol phosphorylcholine and synthesis method, which is applied in the direction of phosphorus organic compounds, chemical instruments and methods, compounds of group 5/15 elements of the periodic table, etc., can solve the problems of unsynthesized method reports and achieve high-efficiency purity Effect
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Embodiment 1
[0030] Synthesis of Compound 3
[0031] Add 89g of dimethylethanolamine and 150g of polyphosphoric acid into the reaction flask, raise the temperature to 150°C for 8 hours, monitor the reaction by GC, stop heating until there is no dimethylethanolamine. Add 2000g of pure water to dissolve, cool down to room temperature, add calcium carbonate / calcium hydroxide to adjust the pH to about 12, filter to remove excess calcium hydroxide, concentrate the filtrate to dryness, add 500g of absolute ethanol to beat to obtain 150g of compound 3 as a solid.
[0032] Synthesis of compound 1
[0033] Take 150g of compound 3, 200g of pure water, and 100g of potassium carbonate into a reaction flask, heat up to 65°C, react for 1 hour, cool down to 30°C, filter, and concentrate the filtrate to dryness. Add 450g of absolute ethanol, 110g of R-chloroglycerin, and reflux at 80°C for 15h. Cool to room temperature and filter. The filtrate was concentrated to dryness, and 20 g was separated through...
Embodiment 2
[0035] Synthesis of Compound 3
[0036] Add 89g of dimethylethanolamine and 150g of polyphosphoric acid into the reaction flask, raise the temperature to 140°C and react for 8 hours, monitor the reaction by GC, stop heating until there is no dimethylethanolamine. Add 2000g of pure water to dissolve, cool down to room temperature, add calcium chloride / calcium hydroxide to adjust the pH to about 12, filter to remove excess calcium hydroxide, concentrate the filtrate to dryness, add 500g of absolute ethanol to beat to obtain 146g of compound 3 as a solid.
[0037] Synthesis of compound 1
[0038] Take 146g of compound 3, 200g of pure water, and 100g of potassium hydroxide into the reaction flask, heat up to 65°C, react for 1 hour, cool down to 20°C, filter, and concentrate the filtrate to dryness. Add 450g of methanol, 110g of R-chloroglycerin, and reflux at 70°C for 15h. Cool to room temperature and filter. The filtrate was concentrated to dryness, and 25 g was separated thro...
Embodiment 3
[0040] Synthesis of Compound 3
[0041] Take 89g of dimethylethanolamine and 150g of polyphosphoric acid into the reaction flask, raise the temperature to 130°C and react for 8 hours, monitor the reaction by GC, stop heating until there is no dimethylethanolamine. Add 2000g of pure water to dissolve, lower the temperature to 30°C, add calcium sulfate / calcium hydroxide to adjust the pH to about 12, filter to remove excess calcium hydroxide, concentrate the filtrate to dryness, add 500g of absolute ethanol and beat to obtain 147g of compound 3 as a solid.
[0042] Synthesis of compound 1
[0043] Take 147g of compound 3, 200g of pure water, and 100g of potassium oxalate into the reaction flask, heat up to 65°C, react for 1 hour, cool down to 30°C, filter, and concentrate the filtrate to dryness. Add 450g of ethanol, 110g of R-chloroglycerin, and reflux at 80°C for 15h. Cool to room temperature and filter. The filtrate was concentrated to dryness, and 30 g was separated throug...
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