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Organosiliconderivativesofphosphorus,arsenic,antimonyandbismuth

Thechemistryofsilylpolyphosphinesiscomplicatedhoweverbynotjustoxygenandwatersensitivity,butalsobytheirtendencytocoupleandexchangeifchlorosubstituted,andtoextensivelyrearrangeinthepresenceofstrongbasesuchasBuLi.Thuscoupling1with2givesaseriesofmonoanddiphosphinesaswellastheexpectedtetraphosphine29(equation44),whileboth1and2witht-BuLigivesmonophosphinederivatives,togetherwiththenoricyclenecagephosphide1(equation45).

Whilethetriphosphine1existsinsolutionasan8:3:1mixtureofisomers30,31and32,respectively,thederivative(R=Bu-t)onlyoccursasthethreoerythroisomer31withaPNMRspectrumshowinganABCpattern.Hydrolysisgivesa2:1mixtureofthreo—threoandthreo—erythroisomersof1.

Thetetraphosphine1(33)resultsfrom1andrearrangesonheatingtocyclopentaphosphineandthediphosphine1(equation46).Insolution,however,itisstablebutpresentasamixtureoffouroffourofthesixpossibleisomersintheratioof11:7:9:3for34,35,36and37,respectively.

Theanalogoust-butyltetraphosphine1resultsfrom(t-BuP)4andpotassiun,followedbysilylation.Itisstabletodisproportionationbelow-30,occurringsolelyastheerythro-(d,l)-erythroisomer35withlargecouplingconstantsJ(PP)duetothetransarrangementofneighbouringt-butylgroups.ThecrystalsteuctureshowstheSi-Pbondstobe228.5pmandthemiddleP—bondof221.4pmtobelongerthanthetwootherP-Pbonds.Hydrolysisgivesa10:5:1mixtureofisomersequivalentto37,36and35ofH(Pbu-t)4H.

VI.CYCLOPOLYPHOSPHINES

A.Cyclotrlphosphlnes

Reacting(t-BuP)3,4withpotassiumgives(t-BuP)2PK,whichgivesthesilylcyclotriphosphine40onsilylation.Methanolylelastheunstablecyclotriphosphine,whichdisproportionatestothecyclotetraphosphine41(equation47).

Cyclotriphosphines43(R=t-Bu,Cl)resultfromthecondensationof1witht-BuPCl2orPCL3.Intiallytheintermediatetetraphosphine42isproducedwhichgivesthecyclotriphosphineoneliminationofCH3SiCl(equation48).

B.Cyclotetraphosphines

Th