Tris chlorodimethylsilyl methylsilane

It is essential to use sublimed A1C13 in this preparation. This may either be obtained commercially (Merck-Schuchardt, Germany) or prepared by sublimation of AIC13 (99% Aldrich) under nitrogen at atmospheric pressure at 185-195°C (recommendation by the checker). Furthermore, the trisilylsilane starting material should be free of any traces of water (if necessary, drying over Na2S04 is recommended). 

The product is a colorless, air- and highly moisture-sensitive solid which has to be handled under an inert gas atmosphere (Schlenk line or glove box). It is soluble in ethers, chloroform, toluene, and acetone. The NMR spectrum (CDC13) exhibits two singlets at 5 0.33 (3H) and 0.62 (18H) (external tetra-methylsilane, TMS). 13C NMR (CDC13) 5 -13.4, 4.5. 

Diethyl ether is dried over sodium benzophenone and is freshly distilled under argon immediately before use. The reaction product is extremely sensitive to moisture and should be handled under an inert gas atmosphere. 

FACILE SYNTHESIS OF ISOMERICALLY PURE cis-DICHLORODIAMMINEPLATINUM(II), CISPLA TIN 

Submitted by VADIM YU. KUKUSHKIN, AKE OSKARSSON, LARS I. ELDING, and NICHOLAS FARRELL  

The colorless crystals (mp 64°C) are air and moisture sensitive. They are highly soluble in ethers, aliphatic and aromatic hydrocarbons, and chloroform. The NMR spectrum (CDCI3) exhibits three singlets at — 0.05 (3H), 0.28 (18H), and 1.16 (27H) (external tetramethylsilane, TMS). NMR (CDCI3) d -13.6, 4.6, 34.0, 51.2. 

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Tris(chlotodimediylsilyl)methylsilane. See Tiisi-lane, l,3-dichloro-2-(chlorodimethylsilyl)-l,lA3,3-pentamethyl-, [107792-64-3] Tris[2-(l,4-diisoiHopylimidazolyl)]phosphine, See ITMmidazole, 2,2, 2"-[diosphinidyne-tiis[l,4-lns(l-methylethyl)-, [160985-99-9] Tiisilane, l,3-dichloio-2-(chlorodimethyIsilyl)-1,1,2,33-pentamethyl-, [107792-64-3], 32 138-139... 

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