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a titre de composés dihalogénosilanes préférentiels, on peut citer les dichlorodiméthylsilane, dichlorodiéthylsilane, dichlorodiphénylsilane, dichlorophénylméthylsilane, dichlorovinylméthylsilane.
dichlorodimethylsilane, dichlorodiethylsilane, dichlorodiphenylsilane, dichlorophenylmethylsilane and dichlorovinylmethylsilane may be mentioned as preferred dihalosilane compounds.
Ultimo aggiornamento 2014-12-03
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28,6 g (113 mmol) de dichlorodiphénylsilane en solution dans 100 ml de thf anhydre sont alors introduits goutte a goutte sous reflux.
28.6 g (113 mmol) of dichlorodiphenylsilane in solution in 100 ml of anhydrous thf are then introduced, dropwise with reflux.
Ultimo aggiornamento 2014-12-03
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mp = 139-140°c rf (dans le toluène) = 0,4 rmn¹h (cdcl₃) : 0,2 (6h,s) ; 0,5-1,9 (6h,q.l.,¹ j bh = 48,6) ; 1,8 (2h,t, j = 13,5) ; 2,39 (2h,d.d., j = 13,8; j = 18,2); 3,8 (6h,s); 6,95-8,18 (18h,m) rmn¹³c (cdcl₃) : 11,14 (d, j =27); 55,23 (s); 111,05 (s); 117,76-161,36 rmn³¹p (cdcl₃) : + 12,4 (d.m., j =56) ir (kbr) : 1017; 1074; 1105; 1130; 1249; 1276; 1431; 1478; 1589; 2365 (b-h); 2403; 2972 (c-h); 3052. analyse pour c₃₀h₄₀o₂¹¹b₂p₂si calculé trouvé masse 544,2459 544,2435 % c 66,17 66,06 % h 7,35 7,42 exemple 11 (r,r)-bis[(2-naphtyl phényl phosphino)méthyl]diphénylsilyl-diborane en procèdant selon les modalités décrites à l'exemple 7 ci-dessus, on obtient à partir de (s)-(méthyl 2-naphtyl phényl phosphine) borane et de dichlorodiphénylsilane le produit attendu avec un rendement e.e. de 100 % après recristallisation du mélange hexane-propanol 1/1 (v/v).
m.p.=139 (cdcl.sub.3): 0.2 (6h, s); 0.5-1.9 (6h, qb, .sup.1 j.sub.bh =48.6); 1.8 (2h, t, j=13.5); 2.39 (2h, dd, j=13.8, j=18.2); 3.8 (6h, s); 6.95-8.18 (18h, m) .sup.13 c nmr (cdcl.sub.3): 11.14 (d, j=27); 55.23 (s); 111.05 (s); 117.76-161.36 .sup.31 p nmr (cdcl.sub.3): +12.4 (dm, j=56) ir (kbr): 1017; 1074; 1105; 1130; 1249; 1276; 1431; 1478; 1589; 2365 (b--h); 2403; 2972 (c--h); 3052 ______________________________________analysis for: c.sub.30 h.sub.40 o.sub.2.sup.11 b.sub.2 p.sub.2 si calculated found______________________________________molecular weight 544.2459 544.2435% c 66.17 66-06% h 7.35 7.42______________________________________ example 11 (r,r)-bis[(2-naphthylphenylphosphino)methyl]diphenylsilyl-diborane if the starting materials are (s)-(methyl-2-naphthylphenylphosphine)-borane and dichlorodiphenylsilane, the expected product is obtained with an e.e. of 100%, after recrystallization from a hexane/propanol mixture (1/1 v/v), by following the modalities described in example 7 above.
Ultimo aggiornamento 2014-12-03
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