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1、About216–224g.(1.62–1.68moles)ofpowderedanhydrousaluminumchlorideisaddedtoa1Lthree-neckedflask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68moles)的无水三氯化铝。Whilethefree-flowingcatalystisstirred(Note3),81g.(0.67mole)ofacetophenoneisaddedfromthedroppingfunnelinaslowstreamoveraperiodof20–30minutes.自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。Considerableheatisevolved,and,ifthedropsofketonearenotdispersed,darkeningorcharringoccurs.放热反应，假如滴加的酮不能被分散，就会变黑或是碳化。Whenaboutone-thirdoftheacetophenonehasbeenadded,themixturebecomesaviscousball-likemassthatisdifficulttostir.当三分之一的乙酰苯被滴加，反应混合物变成一个很难搅拌的粘性的球状团块。Turningofthestirrerbyhandormorerapidadditionofketoneisnecessaryatthispoint.在这时，改用手动搅拌或快速滴加酮是非常必要的。Theadditionofketone,however,shouldnotbesorapidastoproduceatemperatureabove180°.然而，速度不能太快，当反应温度超过180℃时。Neartheendoftheaddition,themassbecomesmoltenandcanbestirredeasilywithoutbeingeitherheatedorcooled.Themoltenmass,inwhichtheacetophenoneiscomplexedwithaluminumchloride,rangesincolorfromtantobrown.当快滴加完时，团块开始融化，表明苯乙酰已经和三氯化铝混合完全，颜色也逐渐从黄褐色变为棕色。Bromine(128g.,0.80mole)isaddeddropwisetothewell-stirredmixtureoveraperiodof40minutes(Note4).在40分钟内在搅拌下把溴缓慢滴加到混合物中。Afterallthebrominehasbeenadded,themoltenmixtureisstirredat80–85°onasteambathfor1hour.溴滴加完后，熔融混合物在80-85℃蒸气浴下搅拌1小时。Thecomplexisaddedinportionstoawell-stirredmixtureof1.3l.ofcrackediceand100ml.ofconcentratedhydrochloricacidina2-l.beaker(Note6).反应物加入到1.3L碎冰和100ml浓盐酸的混合物中在2L的烧杯中混合均匀。Partofthecoldaqueouslayerisaddedtothereactionflasktodecomposewhateverpartofthereactionmixtureremainsthere,andtheresultingmixtureisaddedtothebeaker.把部分的冰水层加入到烧瓶中洗涤残留物，然后合并到烧杯中。Thedarkoilthatsettlesoutisextractedfromthemixturewithfour150-ml.portionsofether分四次把深色的油从混合物中用150ml萃取出来。Theextractsarecombined,washedconsecutivelywith100ml.ofwaterand100ml.of5%aqueoussodiumbicarbonatesolution,driedwithanhydroussodiumsulfate,andtransferredtoashort-neckeddistillationflask.合并萃取液，用100ml水和100ml5%的小苏打洗涤，用无水硫酸钠干燥。Theetherisremovedbydistillationatatmosphericpressure,andcrude3-bromoacetophenoneisstrippedfromafewgramsofheavydarkresiduebydistillationatreducedpressure.乙醚在常压下蒸馏，微量的溴苯乙酮通过减压蒸馏的方法从大量深色残渣中被分离出来。Thecolorlessdistillateiscarefullyfractionatedtoobtain94–100g.通过分馏，得到无色的流出液94-100g2、反应式：3、2-Methyl-4-ethoxalylcyclopentane-1,3,5-trione.Asolutionofsodiumethoxideispreparedina2-l.three-necked,round-bottomedflaskfittedwithamercury-sealedstirrer,arefluxcondensercarryingadryingtube,andastopperbytheadditionof69.0g.(3moles)ofsodiumto950ml.ofabsoluteethanol.69.0g（3mol）钠和950ml无水乙醇在配有干燥回流冷凝管和汞封搅拌器的2L三口圆底烧瓶中制备乙醇钠。Thesolutioniscooledto0–5°inanicebathandstirred.溶液在0-5℃下冰浴搅拌。Thestopperisreplacedbyadroppingfunnel,andacoldmixture(5–15°)of108g.(1.50moles)offreshlydistilled2-butanoneand482g.(3.30moles)ofdiethyloxalate(Note1)isaddedgraduallyoveraperiodof30minutes.瓶塞用分液漏斗取代，108g（1.5mol）的丁二酮和482g（3.3mol）的乙二酸二乙酯在5-15℃下低温混合，在30分钟内逐步滴加到溶液中。Aftertheadditioniscomplete,thethick,orange-redmixtureisallowedtowarmwithcontinuedstirringtoroomtemperature,heatedunderrefluxfor30minutes,andcooledagainto0°inanicebath.完全加入后，橘红色的粘稠物继续搅拌至室温，加热回流30分钟后在冰浴中冷却至0℃。Themixtureisdecomposedbystirringwith165ml.ofsulfuricacid(1:1byvolume)addedinportions.将165ml浓硫酸（体积比1:1）在搅拌加入，分解混合物。Thesodiumsulfateformedisfilteredbysuctionandwashedwithethanol(150–200ml.)(Note2).硫酸钠抽滤后用乙醇（150–200ml）洗涤。Thewashingsandfiltratearecombinedandconcentratedbyevaporation.合并滤液和洗涤液后蒸发浓缩。Theyellowishbrownproductwhichaccumulatesbyslowcrystallizationiscollectedbyfiltration,washedwithsmallquantitiesofice-coldwater,anddriedinair.过滤缓慢析出的棕黄色产品用小剂量的冰水洗涤后在空气中干燥。Thecrudeproductweighs140–150g.粗产品140-150g。Furtherevaporativeconcentrationofthemotherliquorfollowedbycoolingfurnishesanadditional40–50g.oftheketoester,此外将母液用冷冻蒸发浓缩后又得到40-50g的酮酯。bringingthetotalyieldto180–200g.(53–59%)产品总共180-200g（产率53-59%）(Note2).Thiscrudematerial(m.p.120–130°)isusedinthenextstep.粗品（熔点120–130℃）用于下一步中ApuresamplecanbeobtainedbycrystallizationfromethylacetateaftertreatmentwithNoritactivatedcarbon,m.p.160–162°.纯品是经过活性炭处理后在乙酸乙酯中结晶得到，熔点160–162℃。Theprocedurefor2-pyrrolealdehyde2-吡咯甲醛Ina3-l.three-neckedround-bottomedflask,fittedwithasealedstirrer,adroppingfunnel,andarefluxcondenser,isplaced80g.(1.1moles)ofdimethylformamide(Note1).在配有封闭搅拌器、滴液漏斗和冷凝回流装置的三口圆底烧瓶中放入80g（1.1mol）的二甲基甲酰胺。Theflaskisimmersedinanicebath,andtheinternaltemperatureismaintainedat10–20°,while169g.(1.1moles)ofphosphorusoxychlorideisaddedthroughthedroppingfunneloveraperiodof15minutes.烧瓶浸入冰浴中，内部温度保持在10-20℃，169g（1.1mol）的磷酰氯通过滴液漏斗在15分钟内滴加。Anexothermicreactionoccurswiththeformationofthephosphorusoxychloride-dimethylformamidecomplex.放热反应生成磷酰氯二甲基甲酰胺化合物。Theicebathisremoved,andthemixtureisstirredfor15minutes(Note2).移去冰浴，在搅拌15分钟。Theicebathisreplaced,and250ml.ofethylenedichlorideisaddedtothemixture.重新再冰浴下加入250ml的二氯乙烯。Whentheinternaltemperaturehasbeenloweredto5°,asolutionof67g.(1.0mole)offreshlydistilledpyrrolein250ml.ofethylenedichlorideisaddedthroughacleandroppingfunneltothestirred,cooledmixtureoveraperiodof1hour.当内部温度降到5度时，把67g（1.0mol）新蒸馏的吡咯加入到250二氯乙烯中，通过滴液漏斗在1小时内低温下边搅拌边滴加。Aftertheadditioniscomplete,theicebathisreplacedwith