- 1、本文档共3页,可阅读全部内容。
- 2、原创力文档(book118)网站文档一经付费(服务费),不意味着购买了该文档的版权,仅供个人/单位学习、研究之用,不得用于商业用途,未经授权,严禁复制、发行、汇编、翻译或者网络传播等,侵权必究。
- 3、本站所有内容均由合作方或网友上传,本站不对文档的完整性、权威性及其观点立场正确性做任何保证或承诺!文档内容仅供研究参考,付费前请自行鉴别。如您付费,意味着您自己接受本站规则且自行承担风险,本站不退款、不进行额外附加服务;查看《如何避免下载的几个坑》。如果您已付费下载过本站文档,您可以点击 这里二次下载。
- 4、如文档侵犯商业秘密、侵犯著作权、侵犯人身权等,请点击“版权申诉”(推荐),也可以打举报电话:400-050-0827(电话支持时间:9:00-18:30)。
10MURRAYSENKUSVol.68
8-Nitro-isobutyloxy-dihydro-cxP.dicycloentadiene.-pouredintohotwater.Theoillayerwasseparatedand
Borontrifluoride-diethylether(409.)wasagdeddropwisewashedthoroughlywithhotwaterandsodasolution.
toastirredsolutionof178.5g.of2-nitro-isobutylalcohol,Thewashedoilwasdried,mixedwith1%ofitsweightof
198g.ofdicycFpentadieneand200cc.ofethylenedi-drysodiumcarbonateanddistilledinvacuo.Thefraction
chlorideat50.Thetemperaturewasmaintainedatboilingat140-150(1mm.)wasapaleyellowoil.The
60-55bycoolingwithicewater.Thetimerequiredforyieldwas98g.Onstandingitsolidifiedtoacrystalline
theadditionwasthirtyminutes.AftertheexothermicmasswhichafterrecrystallizationfrommethanolTiththe
reactionhadceased,themixturewaswarmedforsixhoursaidofNoriteformedcolorlesscrystals,m.p.70-71.
at40-50thencooled,washedwithwateranddilutesoda
solution,followedbyawaterwash.Theproductaftersummary
dryingyielded212g.ofthecrudenitroetherasacolorless1.Alcoholsandphenolsaddtodicyclopenta-
oilboilingat1.60-180(5mm.).Uponrefractionationdieneinthepresenceofacidiccatalysts(BF8or
thisgave169g.ofthepureproductboilingat136-137
(0.4mm).H2S04)toyieldrearrangedunsaturatedethers,
Phenoxy-dihydro-ero-dicyc1opentadiene.-Toastirredwhicharederivativesofhydroxy-dihydro-cxo-
mixtureof132g.ofdicyclopentadieneand94g.ofphenoldicyclopentadiene.
therewasaddeddropwiseduringthecourse
文档评论(0)