藥物合成反應(yīng)(聞韌_第三版)課后翻譯

1、1、About216–224g.(1.62–1.68moles)ofpowderedanhydrousaluminumchlideisaddedtoa1Lthreeneckedflask.在1L的三口燒瓶中加入大約216224g(1.62–1.68moles)的無(wú)水三氯化鋁。Whilethefreeflowingcatalystisstirred(Note3)81g.(0.67mole)ofacetophenoneisaddedfrom

2、thepingfunnelinaslowstreamoveraperiodof20–30minutes.自由流動(dòng)的催化劑邊攪拌邊用滴液漏斗緩慢滴加81g苯乙酰。Considerableheatisevolvedifthesofketonearenotdisperseddarkeningringoccurs.放熱反應(yīng)，假如滴加的酮不能被分散，就會(huì)變黑或是碳化。Whenaboutonethirdoftheacetophenonehasbee

3、naddedthemixturebecomesaviscousballlikemassthatisdifficulttostir.當(dāng)三分之一的乙酰苯被滴加，反應(yīng)混合物變成一個(gè)很難攪拌的粘性的球狀團(tuán)塊。Turningofthestirrerbyhmerapidadditionofketoneisnecessaryatthispoint.在這時(shí)，改用手動(dòng)攪拌或快速滴加酮是非常必要的。Theadditionofketonehoweversho

4、uldnotbesorapidastoproduceatemperatureabove180.然而，速度不能太快，當(dāng)反應(yīng)溫度超過(guò)180℃時(shí)。Neartheendoftheadditionthemassbecomesmoltencanbestirredeasilywithoutbeingeitherheatedcooled.Themoltenmassinwhichtheacetophenoneiscomplexedwithaluminum

5、chliderangesincolfromtantobrown.當(dāng)快滴加完時(shí)，團(tuán)塊開(kāi)始融化，表明苯乙酰已經(jīng)和三氯化鋁混合完全，顏色也逐漸從黃褐色變?yōu)樽厣romine(128g.0.80mole)isaddedwisetothewellstirredmixtureoveraperiodof40minutes(Note4).在40分鐘內(nèi)在攪拌下把溴緩慢滴加到混合物中。Afterallthebrominehasbeenaddedthemo

6、ltenmixtureisstirredat80–85onasteambathf1hour.溴滴加完后，熔融混合物在8085℃蒸氣浴下攪拌1小時(shí)。Thecomplexisaddedinptionstoawellstirredmixtureof1.3l.ofcrackedice100ml.ofconcentratedhydrochlicacidina2l.beaker(Note6).反應(yīng)物加入到1.3L碎冰和100ml濃鹽酸的混合物中在2

7、L的燒杯中混合均勻。Partofthecoldaqueouslayerisaddedtothereactionflasktodecomposewhateverpartofthereactionmixtureremainstheretheresultingmixtureisaddedtothebeaker.把部分的冰水層加入到燒瓶中洗滌殘留物，然后合并到燒杯中。Thedarkoilthatsettlesoutisextractedfrom

8、themixturewithfour150ml.ptionsofether分四次把深色的油從混合物中用150ml萃取出來(lái)。Theextractsarecombinedwashedconsecutivelywith100ml.ofwater100ml.of5%aqueoussodiumbicarbonatesolutiondriedwithanhydroussodiumsulfatetransferredtoashtneckeddisti