ChemicalBook CAS DataBase List bis(2-methoxyphenyl)-oxophosphanium

bis(2-methoxyphenyl)-oxophosphanium synthesis

7synthesis methods

Product Name:bis(2-methoxyphenyl)-oxophosphanium
CAS Number:71360-04-8
Molecular formula:C14H15O3P
Molecular Weight:262.24

100-66-3 Synthesis

100-66-3
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71360-04-8
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Yield:71360-04-8 97.37%

Reaction Conditions:

Stage #1: methoxybenzenewith n-butyllithium;N,N,N,N,-tetramethylethylenediamine;diethyl phosphonate in diethyl ether at -20 - 30; for 5 h;
Stage #2: with diethyl phosphonate in diethyl ether at -20 - 30; for 1 h;Solvent;Temperature;Reagent/catalyst;

Steps:

4.1 (1) Preparation of bis(2-methoxyphenyl)phosphine oxide

Under anhydrous and anaerobic conditions,2.92g of anisole and 3.13g of tetramethylethylenediaminewas added to 20 mL of ether,Cool down to -20°C,16.87mL of n-BuLi solution was added dropwise under temperature control,After the dropwise addition, the temperature was controlled and stirred for 1 h.The temperature was raised to 30 °C and stirred for 4 h.After the tracking detection reaction is complete,Cool down to -20°C,Start temperature control dropwise additionDiethyl phosphite 4.03g,After the dropwise addition was completed, the reaction was incubated for 1 h.heated to 30°C,After the follow-up detection response is completed,cooled to room temperature,The reaction solution was slowly dropped into theice water with 10% hydrochloric acid,Adjust pH to 3,liquid separation, water washing,Recover tetrahydrofuran under reduced pressure,A large amount of solid was precipitated, dried,2.58 g of white bis(2-methoxyphenyl)phosphine oxide were obtained,Purity 98.88%,Yield 97.37%.

References:

CN114106048,2022,A Location in patent:Paragraph 0090; 0092-0093