- Hydrogen bonding Part 38. IR and thermodynamic study of phosphorylcholine chloride calcium salt tetrahydrate and monohydrate
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Vapor pressure vs.H2O content studies demonstrate that phosphorylcholine chloride calcium salt forms two hydrates, a monohydrate and a tetrahydrate, in the range 0-4 mol H2O mol-1 of salt; there is no dihydrate or trihydrate.Equilibrium vapor pressure measurements show that ΔH0 of dissociation per mol H2O lost is greater for the tetrahydrate (16.08 kcal mol-1) than for the monohydrate (12.49 kcal mol-1); the lower stability of the tetrahydrate arises from entropy effects.The IR spetrum of the tetrahydrate is that of a framework clathrate hydrate and suggests that the -PO3 group may act as a very weak hydrogen-bond acceptor.In the monohydrate the -PO3 group is not involved in hydrogen bonding.Neither hydrate contains P-OH bonds.
- Harmon, Kenneth M.,Akin, Anne C.
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- Glycerin phosphatidyl choline preparation method
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The invention discloses a preparation method of glycerinum phosphatidylcholine. The preparation method comprises the following steps: (1) mixing a compound shown in formula (I) and anhydrous sodium carbonate to obtain a mixture M1; (2) placing the mixture M1 and (R)-(-)-3-chlorine-1,2-propanediol in anhydrous ethanol, and carrying out the refluxing to obtain a mixture M2; (3) filtering the mixture M2, carrying out the membrane separation, removing sodium chloride in the mixture M2, and obtaining filter liquid M3; (4) adding zinc chloride into the filter liquid M3, and dissolving the zinc chloride by adding water to obtain a mixture M4; (5) enabling the mixture M4 to flow by ion exchange resin, filtering the mixture M4, obtaining the filter liquid, and preparing the glycerinum phosphatidylcholine; (see the specifications), wherein R is Ca or Mg. By adopting the method, the glycerinum phosphatidylcholine is simple to prepare, and the yield is high, so that an effect of simple preparation method, high synthesis rate and low production cost can be realized.
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Paragraph 0050; 0051; 0052; 0053; 0054; 0055
(2018/04/20)
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- Glycerin phosphatidyl choline preparation method
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The invention discloses a preparation method for glycerophosphatidylcholine. The preparation method comprises the steps: mixing a compound shown in the formula (I) with anhydrous sodium carbonate to prepare a mixture M1; putting the mixture M1 and (R)-(-)-3-chloro-1,2-propylene glycol in anhydrous ethanol for reflux to obtain a mixture M2; after diluting the mixture M2 by 5-10 times, flowing the mixture M2 through first ion exchange resin to obtain a mixture M3; after diluting the mixture M3 by 2-4 times, flowing the mixture M3 through second ion exchange resin to obtain a mixture M4; washing the mixture M4 by 70-90wt% ethanol to obtain a mixture M5; washing the mixture M5 by distilled water to obtain a mixture M6; after flowing the mixture M6 through third ion exchange resin, filtering the mixture M6 to obtain a filtrate so as to obtain the glycerophosphatidylcholine. The formula (I) is as shown in the description, wherein R is Ca2 or Mg2. The effects of simple preparation method, high synthetic ratio and great reduction of production cost are achieved.
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Paragraph 0056-0061
(2017/12/28)
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- Phosphorus chloride of alkali acid radical gallbladder method for preparing calcium salt
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The invention provides a preparation method of calcium phosphorylcholine chloride, and belongs to the technical field of preparing organic phosphorus compound intermediates. The preparation method comprises the following steps of: putting choline chloride and excess phosphorylation agent in a reaction kettle for a condensation reaction, wherein the obtained condensate liquid is phosphorylcholine chloride; firstly, dissolving phosphorylcholine chloride with water, then adding alum and excess calcium hydroxide to the aqueous solution of phosphorylcholine chloride, regulating the pH, generating crystals and precipitating, and carrying out filter pressing to obtain the clear filtrate; adding calcium chloride to the clear filtrate, concentrating until solid is separated out to obtain the concentrated solution, adding ethanol metered by weight to the concentrated solution, separating out crystals, freezing and filtering to obtain the filter cake, then washing the filter cake with ethanol, and drying to obtain the finished product calcium phosphorylcholine chloride. The preparation method provided by the invention has the advantages of saving the energy source, reducing the energy consumption, shortening the production period, improving the yield and reducing the production cost; the content of calcium phosphorylcholine chloride in the finished product is 99% to 102%; the preparation method meets the requirements of industrial green production.
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Paragraph 0045-0047
(2017/02/24)
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