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ChemicalBook CAS DataBase List Etidronic Acid
2809-21-4

Etidronic Acid synthesis

9synthesis methods
-

Yield:2809-21-4 97%

Reaction Conditions:

with (1-acetyloxyethylidene)-1,1-bisphosphonic acid in water at 75 - 110; for 5 h;

Steps:

1 Example 1; Preparation of hydroxyethanediphosphonic acid (HEDP) directly from yellow phosphorus

Add nitrogen to the reactor with agitation and nitrogen ventilation device to remove oxygen to less than 0.5% of the volume of the container, add 248g of yellow phosphorus (molecular weight 123.9, 2mol),The temperature is raised to 105°C, the negative pressure is 0.098MPa to remove water, and then the nitrogen is deoxygenated through the second pass to less than 0.2% of the entire reactor volume.Use high-purity nitrogen to maintain the positive pressure of the reactor at 0.05Mpa, and slowly inject high-purity oxygen 48g (1.5mol) from the bottom at 65 for 2 hours.The rate of oxygen passing is to ensure that the pressure of the reactor does not increase at 65°C. If it increases, the rate of oxygen passing is reduced. Oxygenation ended the heat preservation reaction for 2 hours.After the reaction was completed, 138 g of 87% acetic acid solution (2 mol of acetic acid and 1 mol of water) was added dropwise at 75°C under the premise of stirring. The dropping time was 2 hours.After dripping, heat to 110°C and keep for 3 hours.Add 18g (1mol) of water and keep at 110 for 1 hour, and then flush with steam until the acetic acid in the product is less than 0.5%.Add water until the product mass fraction is 50% and discharge.

References:

CN111116648,2020,A Location in patent:Paragraph 0016-0023

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