ChemicalBook CAS DataBase List Phosphine, ethynyldiphenyl-

Phosphine, ethynyldiphenyl- synthesis

6synthesis methods

Product Name:Phosphine, ethynyldiphenyl-
CAS Number:6104-47-8
Molecular formula:C14H11P
Molecular Weight:210.21

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Yield:6104-47-8 92%

Reaction Conditions:

Stage #1: trimethylsilylacetylenewith ethylmagnesium bromide in tetrahydrofuran;diethyl ether at 20; for 2 h;
Stage #2: chloro-diphenylphosphine in tetrahydrofuran at -10 - 20; for 3 h;
Stage #3: with potassium carbonate in methanol at 20; for 1.5 h;

Steps:

4.2.3 Ethynyl-diphenylphosphane (3)

The synthesis was carried by analogy to lit. [16, 19] fromHC≡CMgBr (7.36 g, 75 mmol) in THF (200 mL) and chorodiphenylphosphane(13.23 g, 60 mmol). The residual oilwas purified by column chromatography (230 g of silicagel, eluent EtOAc, Rf = 0.75) to obtain 2 as a colorless oil,which gradually crystallized yielding a powder (11.61 g,55 mmol, 92% yield), m. p. 35 °C. The spectroscopic dataagreed with literature data [19].

References:

Marian, Aline;Maas, Gerhard [Zeitschrift fur Naturforschung, B: Chemical Sciences,2020,vol. 75,# 6-7,p. 529 - 536]