ChemicalBook CAS DataBase List TETRAETHYL METHYLENEDIPHOSPHONATE

TETRAETHYL METHYLENEDIPHOSPHONATE synthesis

12synthesis methods

Product Name:TETRAETHYL METHYLENEDIPHOSPHONATE
CAS Number:1660-94-2
Molecular formula:C9H22O6P2
Molecular Weight:288.21

762-04-9
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$10.00/10g

1660-94-2
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$10.00/1g

Yield:1660-94-2 58%

Reaction Conditions:

with sodium in dichloromethane at 0 - 20; for 336 h;Inert atmosphere;

Steps:

Tetraethyl methylenediphophonate 1

The tetraethyl methylenediphosphonate 1 was synthesized by a slightly modified procedure fromliterature1 as follow: A three-necked round bottomed flask equipped with a magnetic stirrer, nitrogensweep and addition funnel was charged with anhydrous dichloromethane (100 mL) and sodium (0.3mol, 6.9 g). A freshly distilled diethylphosphite (0.3 mol, 40 g) was added dropwise at 0°C over 2hours with continuous stirring at 0°C for 48 hours. Then, the reaction the reaction was vigorouslystirred at room temperature for 12 days under nitrogen atmosphere. The obtained blue reaction mixturewas diluted with water (20 mL) and extracted with CHCl3 (3 x 25 mL). The organic layers were driedover Na2SO4 and concentrated under vacuum. The residue was distilled under reduced pressure to provide the tetraethyl methylenediphosphonate 1 in a comparable yield (25 g, 58 %) to that reported byHormi and co-workers.

References:

Yahyaoui, Marwa;Touil, Soufiane;Samarat, Ali [Chemistry Letters,2018,vol. 47,# 6,p. 729 - 731] Location in patent:supporting information

75-09-2 Synthesis