Triphenylbismuth synthesis

Yield:603-33-8 86%

Reaction Conditions:

Stage #1:bromobenzene with lithium in diethyl ether for 0.5 h;Reflux;
Stage #2:bismuth(III) chloride in diethyl ether at 20; for 15 h;

Steps:

3.B B) Preparation of Triphenylbismuthane, Ph₃Bi
5.52 g (795 mmol) of 20 lithium in 250 ml of 14 diethyl ether (Et₂O) are initially introduced in a 1 l three-necked flask with reflux condenser. 44 ml (420 mmol) of 21 bromobenzene are slowly added dropwise via a 250 ml dropping funnel with stirring, so that the diethyl ether boils continuously. When the addition is complete, the grey-brown suspension is heated under reflux for 30 min, and 32.74 g (104 mmol) of 22 bismuth trichloride are subsequently added. The mixture is stirred at RT for 15 h. The suspension is hydrolysed using distilled 23 water with ice-bath cooling and neutralised using a saturated 24 ammonium chloride solution. The organic phase is separated off, and the aqueous phase is extracted twice with Et₂O. The combined organic phases are dried over MgSO₄, and the solvent is removed in a high vacuum. The residue is recrystallised from 80 ml of Et₂O. Repeated decantation and evaporation of the mother liquor and drying in a high vacuum gives 9 triphenylbismuthane in the form of colourless needles. The yield is 39.26 g (89.21 mmol, 86% based on bismuth trichloride). ¹H NMR (CDCl₃), δ, ppm: 7.8 (m, Hortho), 7.4 (m, Hmeta, Hpara).

References:

MERCK PATENT GMBH;HOGE, Berthold Theo;SOLYNTJES, Sven Joerg-Ruediger August;IGNATIEV, Nikolai (Mykola) US2018/273561, 2018, A1 Location in patent:Paragraph 0088; 0089; 0090; 0091

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