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ChemicalBook CAS DataBase List DIMETHYLPHOSPHINE OXIDE
7211-39-4

DIMETHYLPHOSPHINE OXIDE synthesis

14synthesis methods
-

Yield:7211-39-4 88.79%

Reaction Conditions:

in tetrahydrofuran at 0 - 20; for 16 h;Inert atmosphere;

Steps:

1.1J Example 1J Dimethylphosphineoxide

MeMgBr (1.30 mol, 434.46mL) in THF (800mL) was cooled to 0 deg.C. Under the protection of N2, diethyl phosphonate (60.0 g, 434.46 mmol, dissolved in 40mL THF) was added dropwise to the reaction mixture. 2h dropwise additon maintaining the internal temperature not higher than 0 deg.C . After the addition, the reaction mixture was warmed to 20 deg.C and stirred for 14 hours. Solution of potassium carbonate (177 g, was dissolved in 250mL of water) was added to the reaction mixture to quench the reaction. White solid appeared, the mixture was filtered, the filter cake washed with ethanol (100 mL) and washed, the filtrate was concentrated, filtered and concentrated to occur during the solid. Toluene (200 mL) was added to the filtrate, and concentrated to dryness to remove excess water, to give the title compound (30.11 g, 385.78 mmol, 88.79% yield) as a colorless viscous oil.

References:

CN105330698,2016,A Location in patent:Paragraph 0188; 0189; 0190; 0191

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