Pyridine,2-[bis(1-methylethyl)phosphino]-(9CI) synthesis

Yield:745031-93-0 80 %

Reaction Conditions:

Stage #1: 2-pyridylphosphinewith potassium hydroxide in water;dimethyl sulfoxide;
Stage #2: isopropyl bromide in water;dimethyl sulfoxide at 20;

Steps:

3.2.1 General procedure for synthesis of 1 and 2

General procedure: To the solution of the (pyridin-2-yl)phosphine (5.30mmol) in DMSO (15mL), 56% aqueous solution of KOH (15.90mmol) was added dropwise. After 2h, the reaction mixture was cooled between 0 to 10°C and bromoethane or 2-bromopropane (10.60mmol) in DMSO (10mL) was added dropwise over a 1h period. The mixture was allowed to warm to room temperature and was stirred overnight. Degassed water (30mL) was added, the organic layer was separated via canula, and the residuary products were extracted with n-hexane (3×30mL) from aqueous layer. The organic layer was dried over MgSO₄. The solvent was removed by distillation, and the residue was separated by fractional distillation under reduced pressure.

References:

Enikeeva, Kamila R.;Shamsieva, Aliia V.;Kasimov, Airat I.;Litvinov, Igor A.;Lyubina, Anna P.;Voloshina, Alexandra D.;Musina, Elvira I.;Karasik, Andrey A. [Inorganica Chimica Acta,2023,vol. 545,art. no. 121286]