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1、4972A.T.BLOMQUIST,M.PASSER,C.S.SCHOLLENBERGERANDJOSEPHWOLINSKYVol.79Tothissolution,6.6g.(0.1mole)of1-p-Chlorobenzoyl-6-hydroxy-6-p-chlorophenylfulveneclopcutrtdieneWASaddeddropwise.The(VII)wasobtainediii5O',;;yield,1n.p.175-177'(froinitecyelopentadienyllithiuiii'waqstirredforbenzene-he
2、xanemixture).Anal.Calcd.forCl9H12O~CL:15minutes,and14.1g.(0.1mole)ofberizovlchloridewasC,66.5;H,3.5;C1,20.7.Found:C,66.6;H,3.7;C1,addeddropt5iise.Therewasanimmediateformationofa20.5.brightyellowcolor.Stirringnascontinuedfor0.5hr.TheoxazinederivativeVI11wasformedin627;yield.aftertheaddi
3、tionwascomplete,andthereactionmixtureItmeltedat187-188'dec.(from1)enzcne).And.Calcd.washydrolyzedwithdiluteaqueousaceticacid.TheetherforC19HllNOC1?:C,67.1;H,3.3;X,4.1;C1,20.8.layerwasseparatedandtheaqueouslayerextractedtwiceFound:C,67.5;H,3.3;N,4.0;C1,20.5.morewithether.Afterthecombine
4、dextractshadbeenI-o-Chlorobenzoyl-6-hydroxy-6-o-chlorophenylfu~vene(IX)driedoverDrierite,thesolventwasremovedbyevaporationwasformedin26y0yield.Theyellowcrystalswerere-toleaveabrick-redsolid.Afterrecrystallizationfromcrystallizedfromamixtureofethylalcoholandethylglacialaceticacid,whichr
5、emovedcombinedlithiumsalts,acetate.Themeltingpointshowedconsiderablevariationtherewasobtained5.1g.(377,)oforangecrystalsoftheaftereachrecrystallization.Thehighestobservedwasfulvene,m.p.101-102".Themeltingpointwasraisedto146-147.5'.Anal.Calcd.forC1QH12C1202:c,66.5;€1,102-103"byrecrystal
6、lizationfromhexane;A::"264mp3.55;C1,20.6.Found:C,66.7;H,3.6;CL20.6.(logE4.16),282mp(shoulder)(logE4.11),343mp(logE1-p-Nitrobenzoyl-6-hydroxy-6-p-nitrophenylfulvene(X)4.01).Anal.Calcd.forClgH1402:C,83.2;H,5.15;wasobtainedin39'%yield.Recrystallizationfromdi-mol.rvt.,274.3.Found:C,83.5,83
7、.2;H,5.3,5.3;methylformamidegaveyellow,featheryneedles,m.p.248-mol.wt.,290.2.70".A~tnl.Calcd.forC19H12N206:C,62.6;H,3.3.1,4-Diphenylcyclopent[d]-1,2-oxazine(111).~-1solutionFound:C,63.1;H,3.0.Thefulvenealsocouldbere-of1.Og.ofl-benzoyl-6-li~-dro.;v-6-phc~~~lfulve:1eand1.0crystallizetl
