Tetrabutylphosphonium iodide synthesis

Yield: 96%

Reaction Conditions:

at 20 - 100; for 21 h;Inert atmosphere;Darkness;

Steps:

3 2.3 Preparation of tetra(n-butyl)phosphonium iodide
Tri(n-butyl)phosphine (38 mL, 0.15 mol) was slowly added to 1-iodobutane (40 mL, 0.35 mol) under argon. The mixture was stirred for 1 h at RT and then at 100 °C for 20 h. After cooling, the resulting precipitate was washed with diethylether (4 * 50 mL) until a white solid was obtained. Evaporation of residual solvent under vacuum overnight afforded pure nBu₄PI as a white powder (55.6 g, 96%), mp = 95-96 °C. Anal. Found: C, 49.75; H, 9.57. Calc. for C₁₆H₃₆IP: C, 49.74; H, 9.39. δ_H (250 MHz, acetone-d₆) 0.96 (3H, t, ³J 3), 1.55 (2H, m), 1.70 (2H, m), 2.54 (2H, m); δ_P (250 MHz, acetone-d₆) 33.52 (s).

References:

Rodriguez-Zubiri, Mireia;Anguille, Stéphane;Brunet, Jean-Jacques;Daran, Jean-Claude [Journal of Molecular Catalysis A: Chemical,2013,vol. 379,p. 103 - 111]