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ChemicalBook CAS DataBase List Diphenylsilane
775-12-2

Diphenylsilane synthesis

13synthesis methods
A method for preparing diphenylsilane comprises the following steps: adding diphenylchlorosilane in a tetrahydrofuran solution dissolved with a catalyst, carrying out a reaction at the temperature of -10-0 ℃, after the completion of the reaction is monitored by a TLC method, adding the product into an inorganic acid dilute solution under an ice bath condition, and extracting an organic layer, to obtain diphenylsilane. The methods have the advantages that the production processes are greatly simplified, the production costs are low, the purity of the products is high, the content of by-products is low, and the separation is relatively convenient.
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Yield:775-12-2 84.8%

Reaction Conditions:

with lithium aluminium tetrahydride;calcium hydride;zirconium(IV) oxide in diethylene glycol dimethyl ether at 110; for 21 h;Inert atmosphere;

Steps:

4
The 250 mL four-neck round bottom flask was dried, connected to a mechanical stirrer, a spherical condenser tube, a constant pressure funnel and a gas guiding device, and vacuum was used to replace the nitrogen gas three times, while the hot air gun was baked to remove the attached water vapor.Under a nitrogen atmosphere, 9.3 g (0.22 mol) of CaH2, 0.38 g (0.01 mol) of lithium aluminum hydride, 25 mL of diethylene glycol dimethyl ether solvent, and 40 g of ZrO 2 ceramic microspheres (φ = 0.90 mm) were added to the reaction flask.41.5 mL (0.2 mol) of Ph2SiCl2 was added to the constant pressure funnel, and slowly added dropwise to the reaction flask under mechanical stirring.After the completion of the dropwise addition, the mixture was heated to 110 ° C and reacted for 21 hours to obtain the product Ph 2 SiH 2 .According to the integral area of the 1H-NMR spectrum (Fig. 3) of the reaction system, the conversion of the product was 84.8%.

References:

Chinese Academy Of Sciences Chemical Institute;Li Yongming;Chen Yi;Xu Caihong;Wang Xinliang CN108285467, 2018, A Location in patent:Paragraph 0071-0072

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