1of14STANDARDIZEDPHRASEFORREPORT/英文报告标准用语ProcessDescription/工艺描述No.UnitOperationsProcessdescriptioninChineseProcessdescriptioninEnglish1Instrument/Equipmentpreparation仪器/设备准备装有机械搅拌(或磁力搅拌),加料漏斗,温度计(或分水器,干燥管)的3L三口瓶A3Lthree-neckedroundbottomflaskequippedwithmechanicalstirrer(ormagneticstirrer),additionfunnelandthermometer(orDean-Stock;dryingtube)反应中所用的所有瓶子,真空条件下加热30min,氮气吹扫10min。Allflasksusedinthereactionwereheatedundervacuumfor30minutesandpurgedwithnitrogenfor10minutes.将500L高压釜通氮气至0.4~0.5MPa。若0.5~1h内压力无变化,则气密性良好。A500Lautoclavereactorwasfilledwithnitrogentoincreasethepressureto0.4~0.5MPa.Ifthepressurehadnochangewithin0.5~1h,thentheair-tightnessoftheautoclavereactorwasgood.将500L搪瓷釜抽真空到-0.08MPa,再通氮气至常压。重复进行3次。A500Lglass-linedreactorwasevacuatedtolessthan-0.08MPa,thenfilledwithnitrogentonormalpressure.Thiswasrepeatedfor3times.将1000L钛钢釜于60oC用氮气烘6~8h,然后降温到20~25oC。A1000Ltitaniumreactorwasdriedat60oCwithhotnitrogenfor6~8h,thencooledto20~25oC.2Charging/投料Order/顺序向瓶中加入A10ml(1mol),B(2g,2mol)andC(50ml)TheflaskwaschargedwithA(10ml,1mol),B(2g,2mol)andC(50ml)依次加入D(10g,1mol)andE(20ml)D(10g,1mol)andE(20ml)wereaddedinturn向A(10ml,1mol)和B(2g,mol)的C(50ml)溶液(体系或悬浮液)中,依次加入D(10g,1mol)和E(20ml)D(10g,1mol)andE(20ml)wereaddedintoasolution(mixtureorsuspension)ofA(10ml,1mol)andB(2g,mol)inC(50ml)inturnWay/方式氮气保护下,控温20~30oC,通过固体加料漏斗一次性向100L搪瓷釜中加入A(40.0kg,10.0mol)Undertheprotectionofnitrogen,A(40.0kg,10.0mol)wasaddedintoa100Lglass-linedreactorinoneportionviathesolidadditionalfunnelwhilemaintainingthetemperatureat20~30oC控温20~30oC,向500L白钢釜中,分四批加入A(10.0kg,10.0mol),每批2.5kg,间隔时间为5~10minA(10.0kg,10.0mol)wasaddedtoa500Lstainlesssteelreactorinfourportions(2.5kg×4)atintervalof5~10minwhilemaintainingthetemperatureat20~30oC将D(10g,1mol)分批加入,1h加完。D(10g,1mol)wasaddedinportionsduringaperiodof1h.2of14No.UnitOperationsProcessdescriptioninChineseProcessdescriptioninEnglish将D(10g,1mol)分批加入,1h内加完。D(10g,1mol)wasaddedinportionswithin1h.2Charging/投料Way/方式控温20~30oC,用真空向干燥洁净的100L搪瓷釜中抽入114260的乙酸乙酯溶液(外标折算后为50.0kg114260)。Maintainingthetemperatureat20~30oC,solutionof114260inethylacetate(50.0kg114260correctedbywt%)wasaddedbyvacuumtoacleananddried100Lglass-linedreactor控温20~30oC,用氮气压入A(100kg,101mol),开动搅拌,A(100kg,101mol)wasadded(charged)bynitrogenat20~30oCandthenthestirrerwasstarted.控温20~30oC,用真空抽入A(100kg,101mol)Maintainingthetemperatureat20~30oC,A(100kg,101mol)wasadded(charged)byvacuum.控温20~30oC,用泵打入A(100kg,101mol)A(100kg,101mol)wasadded(charged)bypumpwhilemaintainingthetemperatureat20~30oC将正丁基锂或硼烷/四氢呋喃溶液(10ml,1mole,2.5Min己烷),通过管路导入滴加漏斗或A的B溶液中。AsolutionofBuLiorBH3/THF(10ml,1mole,2.5Minhexane)wascannulatedintoadditionfunnelorintoasolutionAinsolventB通过插管,滴加漏斗或针筒,将正丁基锂或硼烷/四氢呋喃溶液(10ml,1mole,2.5Min己烷),通过管路导入滴加漏斗或A的B溶液中,5h加完。AsolutionofBuLiorBH3/THF(10ml,1mole,2.5Minhexane)wasaddedintoasolutionofAinsolventBviacannula,droppingfunnelorsyringeoveraperiodof5h3Adddropwise滴加控温10~15oC,通过50L滴加罐(高位瓶或恒滴)向体系中滴加D(101kg,10mol),滴速为15~20kg/h。D(101g,10mol)wasaddeddropwiseintothemixturethrough(via)50Ladditionalvessel(orcarboyorconstantpressurefunnel)atarateof15~20kg/hwhilemaintainingthetemperatureat10~15oC.控温10oC(或保持微回流或保持内温10~30oC),氮气保护下,(通过加料漏斗或针筒)滴加D(10g,1mol)的E(20ml)溶液。asolutionofD(10g,1mol)inE(20ml)wasaddeddropwise(viaadditionfunnelorsyringe)at10oC(orwhilemaintaininggentlereflux;whilekeepinginnertemperaturebetween10oC~30oC)undernitrogen4Heat升温将体系升温至15~20oC,升温速度5~10oC/hThemixturewasheatedto15~20oCattherateof5~10oC/h.用汽水混合器将体系升温至50~60oC。Themixturewasheatedto50~60oCbythesteam-watermixingheating.5Cool降温将体系降温至15~20oC,降温速度5~10℃/hThemixturewascooledto15~20oCattherateof5~10oC/h.用外浴乙醇/液氮将体系降温至-70~-75oCThemixturewascooledto-70~-75oCbyethanol/liquidnitrogen6Maintain将体系于15~20oC保温搅拌0.5h。Themixturewasstirredat15~20oCfor0.5h。3of14No.UnitOperationsProcessdescriptioninChineseProcessdescriptioninEnglish保温7Reflux回流体系于78~82oC回流3h。Themixturewasrefluxedat78~82oCfor3h.8Exchange/置换控温20~30oC,将氮气通入液面下置换体系10次,每次通氮气至0.2MPa,然后排空至常压;再液面下通氢气置换体系5次,每次通氢气至0.2MPa,然后排空至常压。(高压反应中用到)Themixturewasexchangedwithnitrogenunderliquidlevelfor10times.Thepressurewasincreasedto0.2MPawithnitrogenandpumpeddowntonormalpressureeachtime.Andthenthemixturewasexchangedwithhydrogenunderliquidlevelfor5times.Thepressurewasincreasedto0.2MPawithhydrogenandpumpeddowntonormalpressureeachtime.Duringexchanging,thetemperatureofmixturewascontrolledat20~30oC9React反应Type/类型无溶剂反应:将A(1g,1mol)andB(1g,1mol)溶于溶剂C中,蒸干后,于50oC加热2小时。A(1g,1mol)andB(1g,1mol)weredissolvedinsolventC,evaporatedtodrynessandheatedat50oCfor2h。催化量的反应:于0oC,加入A(20ml,142mmol)和催化量B(1微量或两滴),加入C(4.549g,46.4mmol)的D(120ml)溶液中。A(20ml,142mmol)andcatalyticamount(atraceamountortwodrops)ofBwereaddedintoasolutionofC(4.549g,46.4mmol)inD(120mL)at0oC闷罐反应或封管反应:控温T=40oC,P=0.5MP,A(1g,1mol)的饱和氨水(或其他气体如:一氧化碳、二氧化碳、硫化氢)乙醇(1ml)溶液在50ml封管或闷罐/高压釜中搅拌5小时。AsolutionofA(1g,1mol)inethanol(xml)saturatedwithNH3(orothergassuchas:CO,CO2,H2S)wasstirredunder0.5MPaat40oCfor5hrsina50mlofsealedtubeorautoclave.A(1g,1mol)的饱和氯化氢甲醇(1ml)溶液在20oC搅拌。AsolutionofA(1g,1mol)inmethanol(1ml)saturatedwithHClwasstirredat20oC.控温20oC,向A(1g,1mol)的甲