Bis -/i-chloro

The dimeric species bis-lQi-chioroXCUS-S-T))- ,2,3-tritertbutylpentadiendiyl) rhodium] was reported to undergo a ring-closure accompanied by rearrangement to afford the bis-[( i-chloro) (l-4- n)-l,4,5-tritertbutylcyclopentadi ic))rhodium]. The X-ray crystal structure of one derivative of the product, [Cp((l-4-Ti)-l,4,5-tritertbutylcyclopentadiene))rhodium], (38), was reported. 

As far as the reactions with benzyl chlorides are concerned (74), the oxidative addition of benzyl chloride and substituted benzyl chlorides to palladium atoms yields rj -benzylpalladium chloride dimers. The parent compound, bis(l,2,3-7 -benzyl)di-/i,-chloro-palladium(II), quantitatively adds four molecules of PEts by first forcing the rj -benzyl-iy -benzyl transformation, with subsequent breakage of the Pd-Cl bridges to form trans-bistPEtsKbenzyDchloroPddI). The spectral characteristics of the parent molecule are indicative of the allylic type of bonding. Similar i7 -benzyl compounds were formed from 4-methylbenzyl chloride, 2-chloro-l,l,l-trifluoro-2-phenylethane, and 3,4-dimethylbenzyl chloride. 

Di-/i-chloro-bis(2-acetylacetonylcyclooct-5-en-yl)palladium(II). Di-/i-cbloro-bis(methoxydicyclopentadiene)diplatinum(II). 

Di-/i-chloro-bis(7)4-1,5-cyclooctadiene)dirhodium(l), [RhCl(l,5-C8Hi2)]2, has been prepared in 60% yield by reducing rhodium trichloride hydrate in the presence of excess olefin in aqueous ethanol.1 In the present preparation the yield has been greatly increased (to 94%). Two related complexes, [RhCl(l,5-C6Hio)]22 and [RhCl(C6H12)2]2, are similarly prepared in high yield from 1,5-hexadiene and 2,3-dimethyl-2-butene, respectively. 

RuCls MH2O is a nonstoichiometric material that may differ from one supplier to the other. The complex [Ru(H20)6] is in some cases an alternative precursor," but is difficult to prepare. We wish to present an improved synthesis of di-/i-chloro(dichloro)bis(77 77 -2,7-dimethylocta-2,6-diene-l,8-diyl)diruthenium and its application as a versatile precursor for Ru(ll) complexes with 77 -dienyl ligands. ... 

Di-/i-chloro(dichloro)bis[77 -T7 -2,7-dimethylocta-2,6-diene-l,8-diyl)diruthenium (compound A) is a purple crystalline compound, that is indefinitely stable at room temperature under a nitrogen atmosphere. For short periods it can also be handled in air. MS (El) m/z 616 (M + ). In the solid state the product shows symmetry Ci, ° but it exists as a mixture of two diastereomers in solution. It reacts with various Lewis bases L to form the monomers Ru(t7 77 -CioHi6)Cl2L and it shows catalytic activity in ROMP polymerization. ... 

Dimethylpyridine (0.057 g, 0.53 mmol) is added to a dichloromethane (15 mL) suspension of di-/i-chloro-bis[2-(2-pyridinylmethyl)phenyl-C N-]di-palladium(II) (see Section B) (0.15g, 0.24 mmol) in a 50-mL round-bottomed flask. A clear solution, formed immediately, is stirred for 5 h at room temperature. After the solution is concentrated to 5 mL under reduced pressure, addition of diethyl ether (10 mL) produces white crystals. Yield 0.15 g (72%), mp 257 °C (dec under air in a capillary tube). 

In rats receiving a single oral dose of bis(2-chloro-l-methylethyl)ether of 0.0002-300 mg/kg bw, peak blood levels of radioactivity were reached at about 2-4 h. Following administration of a dose of 30 mg/kg bw, elimination was biphasic in rhesus monkeys, with half-lives of 5 h and two days, and monophasic in rats, with a half-life of two days. In rats, total recovery of radioactivity was 75% of an oral dose of the l- C-labelled compound and 90% after an intraperitoneal dose with the 2-i<-labelled compound approximately 20% of the oral dose was exhaled as CO2 in 48 h. Also in rats, urinary excretion of radioactivity accounted for 48% of a 90 mg/kg bw oral dose of the 1- relabelled compound within 48 h and for 60% of a 30 mg/kg bw intraperitoneal dose of the 2- rC-labelled compound within 24 h. Urinary metabolites identified after administration of an oral dose of 90 mg/kg bw of the I - ( -kibcllcd compound to rats were 2-(2-chloro-1-methylethoxy)propanoic acid (17% of the dose) and N-acetyl-5 -(2-hydroxypropyl)-cysteine (approximately 9% of the dose) following an intraperitoneal dose of the 2- 4C-labelled compound, metabolites identified were l-chloropropan-2-ol, propylene oxide and 2-(2-chloro-l-methylethoxy)propanoic acid (lARC, 1986). 

Synthesis (Eisleb (I.G. Farben), 1937, Eisleb (Winthrop), 1939, Smissman and Hite, 1959 Kleemann et al. 1999) the original synthesis involved condensation of benzyl cyanide with A/,A/-bis(2-chloro-ethyl)-A/-methyl-amine, which is a skin irritant and a carcinogen. 

Ether Bis-[2-chloro-1.1 -difluoro-ethyll- E5, II (( I-CH,-COOH + SF4I. 349f. (COOH- -CF2-0-CF2-)... 

Hydrazine 2.2-Bis-[trifluoronneihyl]-1-(I-chloro-trifluoro-elhyliden]-F.lOb,. 428 (Educt)... 

The treatment of o-bis(dimethylchlorostannyl)benzene 188 with fluoride or chloride ions gave in high yield a variety of /i-halo bis(stannyl)-containing complexes shown in Equation (12) <19980M5858>. The reaction is selective toward fluoride ions. Indeed, reaction of the starting complex 188 with fluoride ions leads only to the formation of the /i-fluoro product, while the /i-chloro product has not been detected. 

Angermaier, K., Zeller, E. and Schmidbauer, H. (1994). Crystal structures of chloro(trimethylphosphine)gold(I), chloro(tri-ipropylphosphine)gold(I) and bis(trimethylphosphine)gold(I) chloride. J. Organomet. Chem. 472, 371. 

Bis(>/6-benzene)molybdenum (2 g, 7.94 mmol) in ca. 400 mL of dry benzene is treated with 1.5 mL (18.43 mmol) of allyl chloride which has been freshly distilled from P4O10. The solution is warmed to 45° in a water bath. The solution rapidly turns a red-violet color and small, purple crystals separate. After 1 hr at 40° the solution is cooled to 6° for 30 min and the light-purple supernatant liquid is decanted. The solid is washed with 100 mL of 95 % ethanol and dried in vacuo. The yield of di-/i-chloro-bis[(>/3-allyl)(t/6-benzene)molybdenum(ll)] is 1.5-1.7 g (75-85%). The solid is ground to a fine powder and transferred to a solution of 3 g (11.47 mmol) of triphenyl-phosphine in 100 mL of benzene. The mixture is stirred under reflux for 1 hr, and the red-purple solution is cooled and filtered. One hundred milliliters of 95 % ethanol is added, and the solution is concentrated to a volume of about 75 mL in vacuo. The solution is then cooled to —15° for 1 hr, and the supernatant is carefully decanted. The small, purple crystals are washed with 100 mL of 95 % ethanol and are dried in vacuo. The yield of ( 73-allyl)chloro( 76-benzene)(triphenylphosphine)molybdenum is 2.4 2.8 g (60-70% yield based on bis( /6-benzene)molybdenum). The solid is ground... 

Di-/i-chloro-bis(l,5-cyclooctadiene)diiridium(I), [IrCl(C8H 2)]2, has been prepared in very good yield by previously reported methods1 from H2 IiCl6 or IrCl3-3H20. ... 

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