METHYLENEDIPHOSPHONIC ACID synthesis

6synthesis methods

Product Name:METHYLENEDIPHOSPHONIC ACID
CAS Number:1984-15-2
Molecular formula:CH6O6P2
Molecular Weight:176

1660-94-2 Synthesis

1660-94-2
187 suppliers
$10.00/1g

1984-15-2
197 suppliers
$23.00/100mg

Yield:1984-15-2 98%

Reaction Conditions:

Stage #1: Tetraethyl methylenediphosphonatewith trimethylsilyl bromide in dichloromethane at 20; for 15 h;Inert atmosphere;
Stage #2: with water in methanol at 20; for 4 h;

Steps:

Methylenebisphosphonate tetramethyl ester (MBP-Me) 4

In a round bottom flask equipped with magnetic stirring bar, 3.5 mmol of 1 and 10 mL of dichloromethane were added. To the solution 42 mmol (12 eq.) of (CH₃)₃SiBr was added, leaving stirring overnight at r.t. under inert atmosphere. The solvent was removed under vacuum and to the crude was added 10 ml MeOH/H₂O. After 4 h reaction, the solvent was removed under vacuum giving the corresponding methylenebisphosphonic acid 7. The latter compound showed characterization spectra in accordance with literature data.

References:

Chiminazzo, Andrea;Sperni, Laura;Fabris, Fabrizio;Scarso, Alessandro [Tetrahedron Letters,2021,vol. 70,art. no. 153012] Location in patent:supporting information