ChemicalBook CAS DataBase List DIPHENYLGERMANE

DIPHENYLGERMANE synthesis

6synthesis methods

Product Name:DIPHENYLGERMANE
CAS Number:1675-58-7
Molecular formula:C12H12Ge
Molecular Weight:228.86

1613-66-7 Synthesis

1613-66-7
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1675-58-7
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Yield:1675-58-7 88%

Reaction Conditions:

with lithium aluminium tetrahydride in diethyl ether; for 6 h;Inert atmosphere;Schlenk technique;Reflux;

Steps:

4.4.4. Diphenylgermane, Ph2GeH2 (9)

Solid LiAlH4 (LAH) (0.96 g, 25.2 mmol, 2.0 eq.) was added portionwiseto the solution of diphenyldichlorogermane, Ph2GeCl2(3.75 g, 12.59 mmol), in ether (40 mL). Then reaction mixture wasrefluxed for 6 h. For the workup the improved procedure fordissolution of products of LAH reductionwas applied, including thesequential dropwise addition of water (0.96 mL, amount in mL isequal to the mass of LAH in g), 15% aq. NaOH (0.96 mL, amount in mL is equal to the mass of LAH in g), water (0.96 mL, amount isequal to the mass of LAH), with time intervals of 10e15 min betweenadditions. This procedure allows to obtain well separatedalumina precipitate, easily removed by filtration or decantation.The inorganic solid was washed with ether (4 20 mL), organicphase was dried over anhydrous MgSO4, and then all volatile materialswere removed under reduced pressure; the residue wasdistilled, giving the target 9 (2.53 g, 88%) as colorless oil, b.p.115e118 C (2mm Hg), b.p. 95 C (1mm Hg) [52]. 1H NMR(400.130 MHz, CDCl3): d 7.61e7.56 (m, 4H), 7.43e7.39 (m, 6H)(aromatic protons), 5.15 (s, 2H, GeH2) ppm. 13C NMR (100.613 MHz,CDCl3): d 135.15 and 128.34 (ortho- and meta-C6H5), 133.99 (ipso-C6H5), 129.07 (para-C6H5) ppm. HRMS (ESI), m/z [M H], calcd.227.8557, found 227.8552.

References:

Zaitsev, Kirill V.;Gloriozov, Igor P.;Oprunenko, Yuri F.;Lermontova, Elmira Kh;Churakov, Andrei V. [Journal of Organometallic Chemistry,2019,vol. 897,p. 217 - 227]