三羟甲基硝基甲烷的合成

三羟甲基硝基甲烷的合成

泰勒（hydrol）-阿农宁（tpm）是一个可以看出是机械的敏感点。它也被用来形成基本的非机构微锁。它是用谷物混合体（hydrol）-椰子（th）、mimosbio（h）、soggrime（hydrol）、nintom（th）、gil和其他材料的混合体。ManyreductionreactionaboutTHAMwerereported1关于tis-hydr统一立法-nitrometh现行Scheme1showedthesynthesisroutsoftris-(hydroxylmethyl)-nitromethane(A)andtris-(hydroxymethyl)-aminomethane(B).1.1indexiege资源Formaldehydesolution(19mL,288mmol)wasaddedslowlyintoasolutionofnitromethane(5.6g,90mmol)inthesolutionofcalciumhydroxide(3mL,0.425mol/L)atpH9beingstirred.Thenthemixturewasstirredat35℃for4h.Theresultingmixturewasadjustedby10%H1.2Twodifferentkindsofcatalyst,RaneyNiandFe(OH)1.2.1si-pcr合作型Toasolutionoftris-(hydroxymethyl)-nitromethane(A)(3g,19.8mmol)inethanol(30mL)anddichloromethane(8mL)wasaddedRaneyNi(0.5g),andthenadded80%N1.2.2fluskwhichcontage,rometh现行Sodiumhydroxide(0.8g)wasaddedintheconicalflaskwhichcontainedFeClTris-(hydroxymethyl)-nitromethane(A)(4g,26mmol)wasdissolvedin30mLethanoland8mLdichloromethane,Fe(OH)2a&bwireconcecontrol见表1IRofcompoundsAandBwereconsistentwiththeknownliterature2.1理想国Themolarratioofnitromethaneandformaldehydewas1∶3astheory,butfromTable1theyieldwaschangedwhilethemolarratioofreactantschanged.Forformaldehyde,selfcondensationundertheconditionofalkalescencywasmade,sotherealquantityshouldbelittlemorethanthetheorythatthenitromethanecouldreactcompletely.ButformTable1,whenthemolarratioofreactantswas1∶3.2,theyieldgotthebest,andmoreformaldehydedidnotaffecttheyield.2.2反应前后比公式Toactivatethenitromethanebeforethereactionbetweennitromethaneandformaldehyde,Ca(OH)2.3通过回归系统回复加数和细胞系统回归并无价格内装,rectinficiens,rectinficiciens,rectinficiens,rectinficiciciens,trille-soincesiptenReactionⅠwasanexothermicreaction.Ifthesolutionofformaldehydewasdroppedsofast,heatwasgivenoutfast,andthetemperatureofthereactionsystemraisedfast.FromTable3,whenthetemperatureover40℃,theyielddecreased.Disproportionreactionwouldreactundertheconditionsofhighertemperatureandstrongalkalescency.Butbelow25℃,itwastoocooltotriggerthereaction.Soitisveryimportanttokeepthereactionatasuitablecondition,fromTable3knownthesuitabletemperatureis30℃-35℃.2.4FromTable4,reactingfor4h,theyieldofTHNMgot91%,anditdidn’tchangeanymore,soafter4hthereactionfinished.2.5质量指标测定ThemolarrateofTHNMandhydrazinehydratewas1∶2astheory,butsomevividhydrogentransgressedofthereactor,andcouldn’treact,soexcessivehydrazinehydratemaygetbetteryield.Thoughtheexperiments,foundthatn(THNM)∶n(hydrazinehydrate)=1∶2.5,theyieldgot50%.2.6rect利益rect赋予whichrectingrectsTemperaturewasfoundmakingalargeeffectintheexperiments.Hydrazinehydratewasdecompoundedwhenitdroppedintothereactionsolutionwhichrefluxingovertemperature,anditcouldn’treactwithnitrocompoundsintime,somorehydrazinehydratewasted.Whenthetemperaturebelow40℃,thereactionwasreactsoslowly,timewastedbutdidnotreducethequantityofhydrazinehydrate.At55℃,gettheproductswithleastreagents.3反应前后合成roctingTheconditionofthesynthesisoftheTHNMwasthatn(nitromethane):n(formaldehyde)=1∶3.2,pH9andstirredfor4hat30℃~35℃,withtheyield91.3%.Reductionreactionwhichusedhydrazinehydrate