67634-27-9Relevant academic research and scientific papers
Process for preparation of substituted aminomethylphosphonic acids
-
, (2008/06/13)
A process is disclosed for the preparation of N-substituted aminomethylphosphonic acids, particularly methylaminomethylphosphonic acid, in high yield and purity with related low production cost using conventional equipment, which comprises the steps of (a) reacting an N-substituted amide with paraformaldehyde in a low molecular weight carboxylic acid to form the N-methylol derivative, (b) reacting the N-methylolamide with PCl3 in excess low molecular weight carboxylic acid and heating to form the phosphonomethyl derivative, (c) hydrolyzing acid chloride and acid anhydride with water, (d) distilling off the low-molecular weight carboxylic acid, (e) hydrolyzing the N-acyl group with water and strong acid catalyst, (f) adding low molecular weight alcohol to crystalline the N-substituted-aminomethyl- phosphonic acid and (g) filtering, and washing the product.
Process for preparation of substituted-aminomethylphosphonic acids
-
, (2008/06/13)
A process is disclosed for the preparation of N-substituted aminomethylphosphonic acids, particularly methylaminomethylphosphonic acid, in high yield and purity with related low production cost using conventional equipment, which comprises the steps of (a) reacting an N-substituted amide with paraformaldehyde in a low molecular weight carboxylic acid to form the N-methylol derivative, (b) reacting the N-methylolamide with PCl3 i n excess low molecular weight carboxylic acid and heating to form the phosphonomethyl derivative, (c) hydrolyzing acid chloride and acid anhydride with water, (d) distilling off the low-molecular weight carboxylic acid, (e) hydrolyzing the N-acyl group with water and strong acid catalyst, (f) adding low molecular weight alcohol to crystallize the N-substituted-aminomethylphosphonic acid and (g) filtering, and washing the product.
NOVEL UNSYMMETRICAL N,N-BIS(METHYLENE)BIPHOSPHONIC ACIDS OF α,ω-DIAMINES. PREPARATION AND CHARACTERIZATION OF BIS(METHYLENE)>-BIPHOSPHONIC ACID AND BIS(METHYLENE)>-BIPHOSPHONIC ACID
Redmore, Derek,Dhawan, Balram
, p. 233 - 238 (2007/10/02)
Reaction of ethylenediamine with phosphorous acid and formaldehyde in molar ratio 1:2:2 gives bis(methylene)>biphosphonic acid (2a) as the major product.Similarly, reaction of hexamethylenediamine with phosphorous acid and formaldehyde in molar ratio 1:2:2 yields bis(methylene)>biphosphonic acid (2b) which is isolated either as bis(methylene>biphosphonic acid (3b) or as bis(methylene)>biphosphonic acid (4b).Removal of the carbobenzoxy group with HBr 3b or the benzoyl group with HCl from 4b gives pure bis(methylene)>biphosphonic acid (2b).All compounds were characterized by 13C NMR, 31P NMR and elemental analysis.
