Lub melting thiab boiling ntsiab lus ntawmNitroso R ntsev (txuas:https://www.bloomtechz.com/chemical-reagent/indicator-reagent/nitroso-r-salt-cas-1189311-71-4.html) nyob ntawm qhov sib txawv me ntsis hauv lawv cov qauv molecular. Feem ntau, lawv cov ntsiab lus melting ntawm kaum mus rau pua pua degrees Celsius. Zoo li ntau cov organic tebchaw, Nitroso R ntsev tsis muaj cov ntsiab lus boiling zoo thiab lawv maj mam decompose thaum rhuab. Qhov ntom sib txawv nrog nws cov qauv thiab muaj pes tsawg leeg. Lawv qhov ntom ntom feem ntau yog nyob nruab nrab ntawm 1 thiab 2 g / cm³, nyob ntawm seb yam xws li qhov hnyav molecular, hloov pauv thiab cov qauv siv lead ua. Nws muaj cov qauv molecular tshwj xeeb, feem ntau pom los ntawm cov pab pawg nitrous oxide (R-NO). Cov qauv no muaj cov nitrous oxide (NO) thiab ib qho kev hloov pauv (R) txuas rau nws. Cov khoom sib txawv yuav ua rau muaj kev hloov pauv hauv lawv lub cev. Thermal stability sib txawv nrog nws cov qauv tshwj xeeb thiab muaj pes tsawg leeg. Feem ntau, lawv decompose thiab hnov mob ntawm qhov kub thiab txias, yog li yuav tsum tau zam kom tsis txhob muaj qhov kub thiab txias kom ruaj khov.
Nitroso R ntsev yog ib chav kawm ntawm cov organic tebchaw uas tuaj yeem ua ke rau ntau txoj hauv kev, nyob ntawm qhov tshwj xeeb R pawg thiab cov tshuaj tiv thaiv. Nov yog qee cov txheej txheem synthesis:
Txoj kev Nitrosylation:
Qhov no yog ib txoj hauv kev siv ntau tshaj plaws rau kev sib txuas ntawm Nitroso R ntsev. Sodium nitrite (NaNO2) reacts nrog cov amine sib raug (R-NH2) nyob rau hauv acidic tej yam kev mob los tsim Nitroso R ntsev. Thaum cov tshuaj tiv thaiv, sodium nitrite yog oxidized rau nitrogen gas, thiab nitrite ion reacts nrog amine los ua Nitroso R ntsev.
Cov hauv qab no yog cov ncauj lus kom ntxaws txog cov txheej txheem nitrosylation:
1. Npaj cov tshuaj tiv thaiv kab mob:
Ua ntej, npaj cov tshuaj tiv thaiv nyob rau hauv qhuav thiab tsis muaj dej. Siv cov kuab tshuaj tsis muaj dej (xws li chloroform, dichloromethane, lossis diethyl ether) thiab desiccants (xws li anhydrous calcium chloride lossis molecular sieves) kom ntseeg tau tias tsis muaj dej noo hauv cov tshuaj tiv thaiv.
2. Ntxiv amine substrate:
Ntxiv qhov xav tau substrate amine rau cov tshuaj tiv thaiv kab mob. Kev xaiv ntawm amine substrate nyob ntawm cov qauv thiab cov khoom ntawm Nitroso R ntsev kom ua ke.
3. Ntxiv acidic tej yam kev mob:
Yuav kom sodium nitrite hnov mob nrog amines los ua Nitroso R ntsev, acidic tej yam kev mob yuav tsum tau muab. Feem ntau siv acidic tej yam kev mob muaj xws li anhydrous HCl acid los yog acetic acid, thiab lwm yam. Ib tug tsim nyog tus nqi ntawm cov kua qaub yog ntxiv rau cov tshuaj tiv thaiv kab mob.
4. Ntxiv sodium nitrite:
Ntxiv sodium nitrite (NaNO2) rau hauv cov tshuaj tiv thaiv kab mob. Feem ntau, sodium nitrite yog ntxiv rau hauv daim ntawv, uas tuaj yeem txiav txim siab raws li cov tshuaj tiv thaiv molar piv thiab tus nqi ntawm cov substrate.
5. Cov tshuaj tiv thaiv cua sov:
Cov tshuaj tiv thaiv kab mob yog rhuab mus rau qhov tsim nyog kub, feem ntau yog nruab nrab ntawm chav tsev kub thiab lub boiling point ntawm reactants. Cov tshuaj tiv thaiv cua sov tuaj yeem txhawb cov tshuaj tiv thaiv ntawm sodium nitrite thiab amine.
6. Lub sij hawm teb:
Lub sij hawm cov tshuaj tiv thaiv yog nyob ntawm qhov tshwj xeeb substrate thiab cov tshuaj tiv thaiv kab mob, thiab feem ntau yog nyob ntawm ob peb teev mus rau hmo ntuj. Kev soj ntsuam ntawm qhov kev nce qib ntawm cov tshuaj tiv thaiv tuaj yeem ua tau thaum lub sijhawm cov tshuaj tiv thaiv, piv txwv li siv nyias txheej chromatography (TLC).
7. Ua haujlwm saum toj no:
Tom qab cov tshuaj tiv thaiv tiav, txias cov tshuaj tiv thaiv kab mob thiab mus ua haujlwm raws li saum toj no. Feem ntau, koj tuaj yeem xaiv los siv cov tshuaj xws li hydrochloric acid lossis acetic acid kom tsis txhob muaj cov kua qaub hauv cov tshuaj tiv thaiv. Tsis tas li ntawd, cov tshuaj tiv thaiv sib tov kuj tuaj yeem ntxuav nrog dilute acid kom tshem tawm impurities.
8. Extraction khoom:
Cov tshuaj tiv thaiv sib tov tau pauv mus rau lub funnel thiab muab rho tawm nrog cov kuab tshuaj qhuav. Ntau cov txheej txheem rho tawm, txhua tus siv cov kuab tshuaj tshiab tshiab, feem ntau yog siv los xyuas kom meej qhov siab tshaj plaws rho tawm ntawm Nitroso R ntsev los ntawm cov tshuaj tiv thaiv sib tov.
9. Cov khoom qhuav:
Hloov cov theem ntawm cov organic rho tawm mus rau qhuav Erlenmeyer flask, thiab ntxiv ib qho tsim nyog ntawm cov kuab tshuaj anhydrous, xws li anhydrous ether lossis acetonitrile. Cov dej hauv cov kuab tshuaj yog tom qab ntawd muab tshem tawm los ntawm kev siv cov desiccant tsim nyog xws li anhydrous sodium chloride lossis molecular sieves.
10. Crystallization:
Cov khoom siv crystalline tau txais los ntawm qeeb evaporation ntawm cov kuab tshuaj. Recrystallization yuav ua tau kom cov khoom purity nce. Qhov kawg tau txais cov khoom siv crystalline yog lub hom phiaj Nitroso R ntsev.
Txoj kev Redox:
Qee cov Nitroso R ntsev tuaj yeem tau txais los ntawm cov tshuaj tiv thaiv redox. Piv txwv li, qhov sib thooj Nitroso R ntsev ntawm choline tebchaw tuaj yeem tsim los ntawm oxidation ntawm nyiaj nitrite (AgNO2). Cov tshuaj tiv thaiv no yuav tsum tau tsim cov tshuaj oxidizing thiab cov kuab tshuaj.
Piv txwv cov kauj ruam yog raws li nram no:
1. Npaj cov tshuaj tiv thaiv: Npaj cov tshuaj tiv thaiv qhuav nyob rau hauv cov dej tsis muaj dej. Siv cov kuab tshuaj anhydrous (xws li dichloromethane, chloroform) thiab desiccants (xws li anhydrous calcium chloride) los xyuas kom meej tias tsis muaj dej nyob hauv cov tshuaj tiv thaiv.
2. Ntxiv substrate: Ntxiv cov substrate yuav tsum tau rau cov tshuaj tiv thaiv kab mob. Qhov kev xaiv ntawm substrate nyob ntawm tus qauv thiab cov khoom ntawm Nitroso R ntsev kom ua ke.
3. Ntxiv cov oxidizing tus neeg saib xyuas lossis txo tus neeg sawv cev: Raws li cov yam ntxwv ntawm lub substrate thiab cov kev xav tau ntawm lub hom phiaj cov tshuaj tiv thaiv, xaiv tus neeg sawv cev oxidizing uas tsim nyog lossis txo tus neeg sawv cev. Feem ntau siv oxidants suav nrog hydrogen peroxide (H2O2), potassium permanganate (KMnO4), thiab lwm yam. Feem ntau siv cov tshuaj txo cov tshuaj muaj xws li sodium sulfite (Na2SO3), sodium hypochlorite (NaClO), thiab lwm yam. Ib qho tsim nyog ntawm oxidizing tus neeg saib xyuas lossis txo tus neeg sawv cev ntxiv rau cov tshuaj tiv thaiv.
4. Ntxiv cov catalyst (optional): Raws li qhov xav tau, ib qho catalyst tsim nyog tuaj yeem ntxiv los txhawb cov tshuaj tiv thaiv. Cov catalysts feem ntau suav nrog kev hloov pauv hlau ntsev, organic acids, thiab lwm yam. Kev xaiv cov catalyst tsim nyog yuav tsum tau ua kom zoo raws li qhov tshwj xeeb cov tshuaj tiv thaiv thiab cov yam ntxwv substrate.
5. Lub sij hawm thiab qhov kub thiab txias: Raws li cov xwm txheej tshwj xeeb, tswj cov tshuaj tiv thaiv lub sij hawm thiab kub. Feem ntau, cov tshuaj tiv thaiv yog nqa tawm ntawm chav tsev kub, tab sis nws yuav tsum tau ua kom sov lossis txias cov tshuaj tiv thaiv, thiab lub sijhawm tshuaj tiv thaiv yuav txawv ntawm ob peb feeb mus rau ob peb teev.
6. Kev tshuaj xyuas cov tshuaj tiv thaiv: Thaum lub sij hawm cov tshuaj tiv thaiv, siv cov kev ntsuam xyuas tsim nyog los saib xyuas qhov kev nce qib ntawm cov tshuaj tiv thaiv. Cov txheej txheem tshuaj ntsuam xyuas muaj xws li infrared spectroscopy (IR), nuclear magnetic resonance (NMR), thiab lwm yam.
7. Neutralize lossis tshem tawm los ntawm cov khoom lag luam: Tom qab cov tshuaj tiv thaiv tiav, raws li cov xwm txheej tshwj xeeb, cov txheej txheem tshuaj tiv thaiv yuav tsum tau ua kom tsis zoo lossis tshem tawm los ntawm cov khoom lag luam. Acid los yog hauv paus tuaj yeem siv los ua kom tsis zoo los ntawm cov khoom hauv cov tshuaj tiv thaiv.
8. Extract cov khoom: Hloov cov tshuaj tiv thaiv sib tov mus rau ib lub funnel thiab extract nrog ib tug tsim nyog tus nqi ntawm cov kuab tshuaj. Ntau cov txheej txheem rho tawm tuaj yeem siv tau, txhua tus siv cov kuab tshuaj tshiab, kom ntseeg tau tias kev rho tawm ntau tshaj ntawm Nitroso R ntsev los ntawm cov tshuaj tiv thaiv sib tov.
9. Qhuav cov khoom: hloov cov theem ntawm cov organic mus rau qhuav Erlenmeyer flask, thiab ntxiv ib tug tsim nyog tus nqi ntawm anhydrous hnyav, xws li anhydrous ether los yog acetonitrile. Cov dej hauv cov kuab tshuaj yog tom qab ntawd muab tshem tawm los ntawm kev siv cov desiccant tsim nyog xws li anhydrous sodium chloride lossis molecular sieves.
10. Crystallization: Cov khoom siv crystalline tau txais los ntawm cov evaporation qeeb ntawm cov kuab tshuaj. Recrystallization yuav ua tau kom cov khoom purity nce. Qhov kawg tau txais cov khoom siv crystalline yog lub hom phiaj Nitroso R ntsev.
Deoxidized alkali hlau txoj kev:
Qee cov Nitroso R ntsev tuaj yeem ua ke los ntawm deoxidized alkali hlau txoj kev. Txoj kev no suav nrog kev ua haujlwm ntawm lub substrate amine nrog alkali hlau (xws li lithium lossis sodium) los tsim cov hlau amine sib xyaw, ua raws li cov tshuaj tiv thaiv oxidation los ntawm oxidizing nitrite kom tau Nitroso R ntsev.
Ua raws li hauv qab no:
1. Npaj cov tshuaj tiv thaiv: Npaj cov tshuaj tiv thaiv qhuav nyob rau hauv cov dej tsis muaj dej. Siv cov kuab tshuaj anhydrous (xws li dichloromethane, chloroform) thiab desiccants (xws li anhydrous calcium chloride) los xyuas kom meej tias tsis muaj dej nyob hauv cov tshuaj tiv thaiv.
2. Ntxiv substrate: Ntxiv nitrite substrate rau cov tshuaj tiv thaiv kab mob. Nitrite substrates tuaj yeem tau txais los ntawm kev ua haujlwm nitric acid nrog cov amines sib xws.
3. Ntxiv alkali hlau txo tus neeg sawv cev: xaiv ib qho tsim nyog alkali hlau txo tus neeg sawv cev, xws li sodium los yog potassium, thiab ntxiv rau cov tshuaj tiv thaiv kab mob. Feem ntau, cov alkali hlau txo tus neeg sawv cev yog ntxiv rau hauv ib qho me ntsis ntau dua li ntawm nitrite substrate los xyuas kom meej qhov txo qis.
4. Lub sij hawm thiab qhov kub thiab txias: Raws li cov kev mob tshwm sim tshwj xeeb, tswj lub sij hawm thiab qhov kub thiab txias. Feem ntau, cov tshuaj tiv thaiv yog nqa tawm ntawm chav tsev kub, tab sis nws yuav tsum tau ua kom sov lossis txias cov tshuaj tiv thaiv, thiab lub sijhawm tshuaj tiv thaiv yuav txawv ntawm ob peb feeb mus rau ob peb teev.
5. Kev tshuaj xyuas cov tshuaj tiv thaiv: Thaum lub sij hawm cov txheej txheem tshuaj tiv thaiv, siv cov kev ntsuam xyuas tsim nyog los saib xyuas qhov kev nce qib ntawm cov tshuaj tiv thaiv. Cov txheej txheem tshuaj ntsuam xyuas muaj xws li infrared spectroscopy (IR), nuclear magnetic resonance (NMR), thiab lwm yam.
6. Neutralize lossis tshem tawm los ntawm cov khoom lag luam: Tom qab cov tshuaj tiv thaiv tiav, raws li qhov xwm txheej tshwj xeeb, cov tshuaj tiv thaiv yuav tsum tau nruab nrab lossis tshem tawm los ntawm cov khoom lag luam. Acid los yog hauv paus tuaj yeem siv los ua kom tsis zoo los ntawm cov khoom hauv cov tshuaj tiv thaiv.
7. Extract cov khoom: Hloov cov tshuaj tiv thaiv sib tov mus rau ib lub funnel thiab extract nrog ib tug tsim nyog tus nqi ntawm cov kuab tshuaj. Ntau cov txheej txheem rho tawm tuaj yeem siv tau, txhua tus siv cov kuab tshuaj tshiab, kom ntseeg tau tias kev rho tawm ntau tshaj ntawm Nitroso R ntsev los ntawm cov tshuaj tiv thaiv sib tov.
8. Qhuav cov khoom: hloov cov theem ntawm cov organic mus rau qhuav Erlenmeyer flask, thiab ntxiv ib tug tsim nyog tus nqi ntawm anhydrous hnyav, xws li anhydrous ether los yog acetonitrile. Cov dej hauv cov kuab tshuaj yog tom qab ntawd muab tshem tawm los ntawm kev siv cov desiccant tsim nyog xws li anhydrous sodium chloride lossis molecular sieves.
9. Crystallization: Cov khoom siv crystalline yog tau los ntawm cov evaporation qeeb ntawm cov kuab tshuaj. Recrystallization yuav ua tau kom cov khoom purity nce. Qhov kawg tau txais cov khoom siv crystalline yog lub hom phiaj Nitroso R ntsev.
Carbon-oxygen exchange method:
Cov pa roj carbon-oxygen pauv cov tshuaj tiv thaiv yog ib txoj kev siv feem ntau rau kev sib txuas ntawm Nitroso R ntsev. Cov txheej txheem cuam tshuam nrog cov pa oxygen atom hauv substrate nrog nitrosylating reagent xws li n-butyl nitrite los tsim cov Nitroso R ntsev.
Qhov no tsuas yog ib qho piv txwv me me ntawm Nitroso R ntsev synthesis txoj kev, yeej muaj ntau lwm tus xaiv los ntawm. Kev xaiv ntawm cov txheej txheem hluavtaws nyob ntawm cov qauv thiab cov khoom ntawm lub hom phiaj xav tau, nrog rau cov kev mob tshwm sim thiab muaj cov tshuaj reagents. Rau cov ncauj lus kom ntxaws txog cov txheej txheem hluavtaws, thov xa mus rau cov ntaub ntawv tseem ceeb ntawm cov khoom siv hluavtaws chemistry lossis nrog tus kws tshaj lij kws tshuaj.