A highly efficient method for the synthesis of chloro‐substituted subphthalocyanines employing a 1 M boron trichloride solution in p‐xylene is described and compared to other previously described results. The substitution reaction of the axial chlorine atom by a phenoxy group has been optimized. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)

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The interaction of chlorohydridotris(triphenylphosphine)ruthenium(il) with NaOH or KOH in tetrahydrofuran, acetone, or t-butyl alcohol leads, depending on conditions, first to red, five-co-ordinate complexes RuH (OH) (PPh,),-(sol) (sol = thf or H,O) secondly to hydroxo-bridged dimers. (PPh,),H(sol) Ru(p-OH),Ru(sol) H(PPh,), (sol = Me,CO, H,O, or ButOH) and thirdly to a tetranuclear complex of stoicheiometry Ru,H,(OH),( PPh,),(CO),-Interaction of dichlorotris(triphenylphosphine)rufhenium (ll) with KOH gives similar compounds, RuCI(0H)-(PPh,),(sol), and {RuCI(OH)(PPh,),(sol)),(sol = H, O or thf) as well as (RuH(OH)(PPh,),(thf)),.The interaction of RuHCI(PP~,)~ with sodium methoxide gives rise to two compounds that are formulated. respectively as having RU-CHO and RU-OCH, groups, The mechanism of decarbonylation of alcohols isdiscussedand the compounds RuH,(CO)(PPh,),*ROH ( R = Me or Et) are synthesised. 1.r. and l H and 31P n.m.r. spectra of the various complexes are given and structures for the compounds proposed on this basis. Department, Imperial College, London SW7 2AY ( PPh3)6 (MeZCO) 2.ALTHOUGH some hydroxo-complexes of ruthenium have been known for nearly 90 years,l-lo no systematic attempts to prepare them have been reported, perhaps on account of the supposed lack of affinity between the hard OHligand and the presumed soft class B metal t No reprints available.

Five new trisiloxane quaternary ammonium compounds were synthesized from hydrotrisiloxane with allyl glycidyl ether to yield the epoxy function. Various amines were then reacted to yield trisiloxane amines which were further reacted to methyl substitute or oxidize the beta-carbons in order to provide thermal stability. These new compounds were employed as melt additives in a nonwoven polypropylene fiber extrusion process to produce, through surface segregation, a new biomaterial with antibacterial properties.

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A mechanistic study of chloroboron subphthalocyanine (SubPc) formation from phthalonitrile and BCl 3 in aromatic solvents such as p-xylene or toluene suggests that rearrangement of the initial phthalonitrile- BCl 3 adduct produces (1 Z )-3-chloro-N-(dichloroboryl)-1 H -isoindol-1-imine 3, following rearrangement of the initial phthalonitrile- BCl 3 adduct. From three molecules of (1 Z )-3-chloro-N-(dichloroboryl)-1 H -isoindol-1-imine 3, by successive addition, the dichlorosubstituted macrocycle 7 is formed. Quantum-chemical computation shows that the postulated elementary reaction steps leading up to the formation of the SubPc-precursor macrocycle are indeed exothermic, or at least kinetically allowed. The formation of the SubPc is concluded by the elimination of chlorine which is probably catalyzed by BCl 3 in a concerted process which might be represented as: dichlorosubstituted macrocycle 7 + BCl 3 → SubPc · Cl + + BCl 4- → SubPc + Cl 2 + BCl 3. The chlorine formed may be photolytically affected if the reaction is carried out under ordinary laboratory lighting (fluorescent lamps), giving rise to a free-radical chain reaction involving the solvent. Alternatively, molecular chlorine may react with aromatic solvents such as toluene and p-xylene in a Friedel-Crafts-type reaction catalyzed by BCl 3. In this way, such solvents which are reactive in both ways can protect the reactant phthalonitrile, the reaction intermediates, and the product SubPc from degradation by chlorination.

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