Preparation of calcium pantothenate
OwnerRobert D. Lekberginventor
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Abstract
Beta-amino propionitrile is hydrolyzed with potassium hydroxide to produce potassium beta alanate, which, upon acidification produces free beta alanine with some potassium sulfate precipitate. The beta alanine solution with residual potassium sulfate is concentrated under vacuum to a thick syrup, shocked with an excess of a selected alcohol to produce a solid mass of beta alanine with the remaining theoretical potassium sulfate. The solid product is converted to calcium beta alanate under anhydrous conditions for reaction with racemic pantoyl lactone to form pure calcium pantothenate and allowing the entrained potassium sulfate to settle out. Contrary to expectations, under these conditions there was no double displacement and the presence of potassium sulfate did not interfere with the reaction.
Claims10
A process for the preparation of calcium pantothenate comprising:
- reacting beta-amino propionitrile with a substantially stoichiometric quantity of potassium hydroxide in aqueous media to produce potassium beta alanate;
- distilling off volatiles produced in the reaction;
- reacting the potassium beta alanate distilland with sulfuric acid to form free beta alanine and a precipitate of potassium sulfate;
- separating the precipitated potassium sulfate and recovering the filtrate;
- distilling the filtrate to remove water and recovering a concentrated filtrate;
- treating the concentrated filtrate with low molecular weight anhydrous aliphatic alcohol to form a precipitate comprising a mixture of beta-alanine and entrained potassium sulfate;
- reacting the beta-alanine and potassium sulfate mixture with calcium methoxide under substantially anhydrous conditions to form calcium beta alanate;
- reacting the calcium beta alanate with racemic pantoyl lactone in the presence of the entrained potassium sulfate under substantially anhydrous conditions to form substantially pure calcium pantothenate;
- and
- separating soluble calcium pantothenate from the remaining potassium sulfate which settles therefrom.
A process for the preparation of calcium pantothenate comprising the steps of:
- reacting beta-amino propionitrile with potassium hydroxide in aqueous media to form potassium beta alanate;
- distilling off volatiles produced in the reaction;
- reacting the potassium beta alanate distilland so produced with sulfuric acid in a minimum amount of water to form free beta-alanine and a precipitate of potassium sulfate;
- separating the precipitated potassium sulfate and recovering the filtrate;
- distilling the filtrate to remove water and recovering a concentrated filtrate;
- treating the concentrated filtrate with an aliphatic alcohol under anhydrous conditions to form a mixture of precipitated beta-alanine and entrained potassium sulfate;
- reacting the beta-alanine and potassium sulfate mixture with calcium methoxide to form calcium beta alanate;
- reacting the calcium beta alanate with pantoyl lactone in the presence of the entrained potassium sulfate under substantially anhydrous conditions to form substantially pure calcium pantothenate;
- and
- separating soluble calcium pantothenate from the insoluble entrained potassium sulfate.
Dependencies are inferred from the claim text.