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ChemicalBook CAS DataBase List 1,3-Bis(diphenylphosphino)propane

1,3-Bis(diphenylphosphino)propane synthesis

9synthesis methods
-

Yield:6737-42-4 80%

Reaction Conditions:

with indium(III) bromide;1,1,3,3-Tetramethyldisiloxane in toluene at 100; for 22 h;Inert atmosphere;Sealed tube;

Steps:

General procedure for the preparation of compounds 2a, 2g and 2h.
General procedure: In a sealed tube containing a solution of the phosphine oxide derivative (5 mmol) in anhydrous toluene (1M) was added InBr3 (1 mol %, 0.05 mmol) and the TMDS (1.5 equiv., 7.5 mmol). The reactionnal mixture was stirred at 100 °C during 7 to 40 h depending on the substrate (the reaction was monitored by 31P NMR). After complete consumption and evaporation of toluene the phosphine was purified by flash chromatography on silica gel with pure cyclohexane) to afford the desired phosphine.

References:

Pehlivan, Leyla;Métay, Estelle;Delbrayelle, Dominique;Mignani, Gérard;Lemaire, Marc [Tetrahedron,2012,vol. 68,# 15,p. 3151 - 3155] Location in patent:supporting information; experimental part

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