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ChemicalBook CAS DataBase List Triphenylphosphine hydrobromide
6399-81-1

Triphenylphosphine hydrobromide synthesis

3synthesis methods
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Yield:6399-81-1 98%

Reaction Conditions:

with hydrogen bromide in 1,4-dioxane;water at 20 - 70; for 12 h;

Steps:


A solution of 48% aqueous hydrobromic acid (1mL, ca. 8.8 mmol) was added dropwise for 1 min to the stirring mixture oftriphenylphosphine (1.05 g, 4 mmol) in dioxane (8 mL) at room temperature, and warmed to70 °C. After the mixture was stirred at 70 °C for 12 h, the mixture was evaporated in vacuo.The residue was washed with ether, and the precipitate was dried in vacuo for 12 h at 40 °C togive 1a•HBr (1.34 g, 98%) as a white solid; 1H NMR (400 MHz, DMSO-d6, 25 C) δ (ppm):7.53-7.59 (m, 6H, ArH), 7.60-7.67 (m, 9H, ArH), 10.60 (brs, 1H, PH). 13C NMR (100 MHz,DMSO-d6, 25 °C) δ (ppm): 128.77 (d, J = 11.4 Hz, Ar), 131.48 (d, J = 9.6 Hz, Ar), 132.05 (d,J = 1.9 Hz, Ar), 132.70 (d, J = 102 Hz, Ar).

References:

Aoyagi, Naoto;Furusho, Yoshio;Endo, Takeshi [Tetrahedron Letters,2013,vol. 54,# 51,p. 7031 - 7034] Location in patent:supporting information

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