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ID:40648077
大小:20.85 KB
页数:5页
时间:2019-08-05
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1、这个你可以甩两眼! Enote操作中可用英文例句反应部分sealedtube封管pressuretankreactor高压釜freshlyprepared新制的Thesuspension悬浮液addedinseveralportion分批加ssaturatedaqueousNaHCO3饱和NaHCO3水溶液GrignardReagents格氏试剂initiatedby引发 Intoa200ml4-neckedroundbottomflaskpurgedandmaintainedwithaninertatmosphereofnitrogen,在充满氮气的200毫升四颈圆底烧瓶中A
2、200mlflaskwaschargedwithasolutionofSMinTHFundernitrogenatmosphere,在充满氮气的200毫升烧瓶中加入SM的THF溶液XXwasaddedviamicrosyringeto….用微量注射器把XX加入到…Theflaskwasevacuatedandflushedthreetimeswithnitrogen,followedbyflushingwithhydrogen.Themixturewasstirred2hatroomtemperatureunderanatmosphereofhydrogen(balloon).
3、反应瓶用氮气置换三次,紧接着通氢气。在氢气环境下(氢气球),室温下混合搅拌2个小时。ThiswasfollowedbytheadditionofasolutionofSM(50g)inH2O(50ml),whichwasaddeddropwisewithstirringat0degreesCin15mins.将50gSM溶于50mL水制成的溶液在0℃条件下滴加到上述混合液中,滴加时间为15分钟。ThissolutionwasslowlytransferredtoasolutionofXXXinanhydrousTHF(20mL).该溶液被慢慢转移到XXX的THF(20mL)溶液
4、中TotheaboveH2(g)wasintroducedin在以上混合液中通入H2气Theabovemixturewasstirredfor1hourat-20degreesC.以上混合物在-20度搅拌1小时Thefinalreactionmixturewasirradiatedwithmicrowaveradiationfor10minsat90degreesC.最终的混合物用微波辐射10分钟在90℃Thereactionmixturewasthenheatedtorefluxfor30min反应液加热回流30分钟Thetemperaturewasincreasedtoro
5、omtemperaturenaturally.自然升温到室温Thereactionmixturewassonicatedatroomtemperaturefor3h.反应混合物在室温下超声3h。Themixturewasheatedfor1.5hrunderrefluxandwaterseparation.混合物在水分离的条件下回流1.5h。ThewaterformedinthereactionwasremovedviaaDean-Starktube反应中形成的水份通过Dean-Stark管除去。 Thetemperatureoftheexternalbathwascarefu
6、llymaintainedbetween-20and-25degreesCduringtheaddition.外面冰水浴的温度要保持在-20℃~-25℃之间。Ozonewasbubbledslowlyintothesolutionuntilthereactionmixtureturnedcolorless;Nitrogenwasthenpassedthroughthesolutiontoremoveanyexcessozone.臭氧被慢慢地鼓泡进入反应液直到反应液变成无色,然后通入氮气来去除多余的臭氧Aftercooledtoroomtemperature,thereactio
7、nmixturewas…冷却到室温后,反应混合物被…Thereactionwascooledto-20degreesC.该反应冷却到-20℃Theresultingsolutionwaskeptundisturbedovernight生成的溶液被静置过夜后处理部分Thereactionmixturewaspouredinto200gofcrushedice.Theisolatedsolidwascollectedandpurifiedbyrecrystalizationwithethanol
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