ChemicalBook CAS DataBase List Tris(2-Methoxyphenyl)phosphine

Tris(2-Methoxyphenyl)phosphine synthesis

5synthesis methods

Product Name:Tris(2-Methoxyphenyl)phosphine
CAS Number:4731-65-1
Molecular formula:C21H21O3P
Molecular Weight:352.36

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Yield:-

Reaction Conditions:

Stage #1:2-bromoanisole with magnesium in tetrahydrofuran for 2 h;Reflux;
Stage #2: with phosphorus trichloride in tetrahydrofuran at -78; for 2 h;

Steps:

5
The preparation of tri(2-methoxyphenyl)phosphorus was carried out in the following manner. 91.1 g (3.75 mol) of magnesium pieces were slowly added to 95 mL (0.75 mol) of 2-bromo-anisol in 2 liters of THF. After intensive reaction, the reaction mixture was heated under reflux for 2 hours to obtain a Grignard reagent. The Grignard reagent was added dropwise to a solution of 17.5 mL (0.2 mol) of PCl₃in 2 liters of THF at -78° C. over 2 hours with stirring. After completion of the dropwise addition, the dry ice/acetone bath was removed, and the reaction material was warmed to room temperature. The reaction material was stirred overnight, and the solvent was removed in a vacuum. The phosphine product was used in a subsequent step without removal.

References:

SK Innovation Co., Ltd.;SK Global Chemical Co., Ltd. US8309779, 2012, B2 Location in patent:Page/Page column 18

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529-28-2 Synthesis