Tris(2-Methoxyphenyl)phosphine synthesis
- Product Name:Tris(2-Methoxyphenyl)phosphine
- CAS Number:4731-65-1
- Molecular formula:C21H21O3P
- Molecular Weight:352.36
578-57-4
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4731-65-1
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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 PCl3 in 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
529-28-2
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4731-65-1
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100-66-3
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13139-86-1
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4731-65-1
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