实验记录模板-反应及后处理.doc

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1、实验名称/TitleSynthesisofC-A项目编号/ProjectNo.___________记录本编号/BookNo.__________上接页数/FromPageNo.N/APurpose:ProviderawmaterialReaction:Substances:Name:Quant.Mol.wt.m.molsEquiv.SourceC-F10gTHF100gPotassiumcarbonate4.5g3-Bromopropene4.2gProcedure:25-AUG-2011指当天做实验的起始日期08

2、:05preparetheexperimentinstrument08:3010g(1.0X)ofC-F,100g(9X-10X)ofTHFand4.5g(0.43X-0.45X)ofPotassiumcarbonatewereaddedintoa500mlflask.Themixturewasstirredat15-25˚Cfor40min.09:104.8kg(0.37X-0.39X)of3-Bromopropenewasaddedintotheflaskat15-25˚C.Themixturewasheated

3、to55˚Candstirredat55-65˚Cfor8hrs.09:40Thereactionwaswarmedover30minfrom28to55˚C.17:40AsamplewastakenanddetectedbyHPLC(No.:HCS13132-33-01)18:35Themixturewascooledto25˚C.Work-up18:40ThemixturewasfilteredthroughaBuchnerfunnelthewetcakewaswashedwith20gofisopropylac

4、etate.19:00Over20min,thefiltratewastransferredbacktoa1Lflask.19:1040g(3.0X-3.2X)ofisopropylacetateand62g(4X-6X)ofwaterwasaddedintotheflask.19:30Themixturewascooledto15˚Cover20min.13.2g(1.0X-1.5X)of0.1MH3PO4solutionwasaddeddropwiseintotheflaskbelow15˚CuntilpH=6滴

5、加、调酸.19:55Over25min,thelayerswereseparated分离,theaqueouslayerwasextracted萃取twicewithisopropylacetate,27g(2.0X-2.5X),29.4g(2.0X-2.5X)inturn.20:15Thecombinedorganiclayerwaswashedwith60g(4X-6X),63g(4X-6X)ofwaterintu有机相用水洗两次，每次用多少量的水都列出来了rn.下接页数/ToPageNo.2复核人/Review

6、edbyXXX日期/DateDD-MMM-YYYY发明人/InventedbyN/AXXX日期25-AUG-2011实验名称/TitleSynthesisofC-A项目编号/ProjectNo.—————记录本编号/BookNo.—————上接页数/FromPageNo.120:30Theorganiclayerwasconcentrated减压浓缩toapproximately26-39ml(2X-3X)underreducedpressurebelow40˚C.21:0075g(5X-6X)ofethanolwa

7、saddedintoflaskandwasconcentratedtoapproximately26-39ml(2X-3X)underreducedpressurebelow40˚C.26-AUG-201108:1060g(4X-5X)ofethanolwasaddedintoa500mlflaskabove.Themixturewasstirredat15-25˚Cfor2hrs.打浆10:30Themixturewasfilteredoff,thewetcakewaswashedwith19g(4X-6X)ofe

8、thanol.10:50Thewetcakewasdriedundervacuumat55-60˚Cfor6hrs真空干燥toget11.91gofintermediateC-A,theyieldwas93%.17:00ThesolidwastakentodetectebyHPLC(NO.:SM101-YQ1126-11273-02-B).Re