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ChemicalBook CAS DataBase List METHYLENEDIPHOSPHONIC ACID

METHYLENEDIPHOSPHONIC ACID synthesis

6synthesis methods
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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

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