54722-12-2Relevant articles and documents
Compound containing phosphine chiral center, organic transition metal complex and preparation method thereof
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Paragraph 0055-0059; 0061-0065; 0067-0071; 0073-0077; 0079.., (2021/07/10)
The invention provides a compound containing a phosphine chiral center, an organic transition metal complex and a preparation method thereof. The preparation method of the compound comprises the following steps: (1) reducing a secondary phosphine oxide 1 into a product secondary phosphine hydrogen 2 by using a reducing agent, wherein the reaction temperature is 20 to 100 DEG C, and the reaction time is 12 to 120 hours; and (2) adding alkyne and the secondary phosphine hydrogen prepared in the step (1) into an organic solvent by using a metal catalyst and a chiral ligand as catalysts to obtain the chiral phosphine compound. The synthesized chiral phosphine compound can be used as a ligand to directly react with transition metal salt to synthesize various organic transition metal complexes. According to the synthesis method disclosed by the invention, secondary phosphine oxide with good stability and low odor is used as a raw material, so that direct use of secondary phosphine with high toxicity and odor for reaction is avoided, and the chiral trivalent phosphine product and the derivative thereof are efficiently and selectively obtained.
A straightforward synthesis of unsymmetrical secondary phosphine boranes
Petit, Christelle,Favre-Reguillon, Alain,Mignani, Gerard,Lemaire, Marc
experimental part, p. 326 - 330 (2011/03/18)
A one-pot procedure for the synthesis of unsymmetrical alkyl-substituted secondary phosphine oxides is described. The sequential addition of N-benzylaniline to a solution of dichlorophenylphosphine and 1-methylimidazole in methylcyclohexane, separating of the protic ionic liquid formed, addition of Grignard reagent followed by hydrolysis gave unsymmetrical secondary phosphine oxides (SPOs) in high yield. The use of ionic liquids in the first step is essential and streamlined the synthesis. Unsymmetrical SPOs could be quantitatively reduced to secondary phosphine using a catalytic amount of Ti(OiPr)4 and tetramethyldisiloxane (TMDS) under mild reaction conditions.
Synthesis of electron-deficient secondary phosphine oxides and secondary phosphines: Bis[3,5bis(trifluoromethyl)phenyl]phosphine oxide and bis[3,5-bis(trifluoromethyl)phenyl]phosphine
Busacca, Carl A.,Lorenz, Jon C.,Sabila, Paul,Haddad, Nizar,Senandyake, Chris H.,Denmark, Scott E.,Regens, Christopher S.
, p. 242 - 261 (2017/09/27)
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