1. Ntxiv phosphorus pentoxide thiab reflux kom txog thaum phosphorus pentoxide tsis tig daj, ces evaporate nyob rau hauv kev tiv thaiv nitrogen;.
2. Ntxiv calcium hydride thiab reflux rau rau mus rau yim teev, ces evaporate nyob rau hauv kev tiv thaiv nitrogen;
3. Tshem tawm dej los ntawm molecular sieve, qhuav lub 4A molecular sieve ntawm li 300 degree rau 6-8 teev, txias nws mus rau chav tsev kub nyob rau hauv nitrogen tiv thaiv, ntxiv rau acetonitrile nyob rau hauv nitrogen tiv thaiv los yog cia nws sawv nyob rau hauv ib tug qhuav qhov chaw. rau ntau tshaj 12 teev.
4. Ntxiv silica gel los yog 4A hom molecular sieve tshem tawm cov dej hauv acetonitrile, ces ntxiv calcium hydride thiab do kom txog thaum cov roj hydrogen tsis tso tawm. Nyob rau hauv txoj kev no, acetic acid tuaj yeem raug tshem tawm, tawm hauv tsuas yog ib qho dej xwb. Tom qab ntawd distilled ntawm qhov sib piv siab reflux, saib xyuas kom tsis txhob ya raws nkag mus. Rau lub hom phiaj no, reflux ntawm calcium hydride. Koj tseem tuaj yeem ntxiv 0.5%-1% phosphorus pentoxide rau lub tshuab nqus dej kom tshem tawm feem ntau ntawm cov dej seem. Kev saib xyuas yuav tsum tau ua kom tsis txhob muaj ntau ntau ntawm phosphorus pentoxide, vim nws yuav tsim cov txiv kab ntxwv polymer.
5. (1) Rau kev tshem tawm cov dej ua ntej, thawj zaug muab acetonitrile rau hauv ib lub thawv, ntxiv 4A molecular sieve (qhuav molecular sieve), thiab muab kaw rau 12 teev.
(2) Distillation. Ncuav cov tshuaj tom qab thawj zaug tshem tawm dej mus rau hauv ib lub thoob-bottomed flask, ntxiv ib tug tsim nyog tus nqi ntawm phosphorus pentoxide, thiab siv ib tug sib nqus stirring rotor. Distilled kom txog thaum cov xim ntawm phosphorus pentoxide tsis tob lawm (feem ntau 5 mus rau 6 teev). Tso cov tshuaj rau hauv lub dispenser (siv lub tshuab ziab plaub hau los ntxuav lub raj mis uas muaj cov tshuaj). Tom qab ntawd, lub raj mis uas muaj cov tshuaj raug kaw thiab txuas nrog rau qhov kawg ntawm lub dispenser. Txuas ntxiv cua sov kom distilled tawm cov tshuaj ntxiv, tawm hauv 100ml. Chav tawm. Lus Cim: Cov tshuaj yuav tsum ua kom npau taws thoob plaws hauv cov txheej txheem.
(3) Cia: Ntxiv cov tshuaj distilled rau qhuav molecular sieves, foob thiab khaws cia deb ntawm lub teeb.
6. Acetonitrile yog infinitely miscible nrog dej thiab cawv, thiab tuaj yeem tsim binary azeotrope nrog dej. Nws muaj pes tsawg leeg thiab azeotropic point yog raws li nram no: Azeotropic point: 77 degrees Celsius (101.33kpa), acetonitrile ntsiab lus 77% (W). Acetonitrile yog lub cev qhuav dej. Txij li thaum acetonitrile thiab Dej yog infinitely soluble nyob rau hauv ib leeg, thiab nws yog ib qho nyuaj rau dehydrate acetonitrile. Acetonitrile thiab dej tuaj yeem tsim ib qho azeotrope, tab sis cov dej tsis tuaj yeem sib cais. Txhawm rau ua kom zoo dua ntxiv, koj tuaj yeem qhuav nws nrog anhydrous calcium chloride ua ntej, tom qab ntawd ntxiv 0.5-1% tsib zaug tom qab pom. Phosphorus oxide (P2O5) yog refluxed thiab ces distilled nyob rau hauv ib txwm siab. Rov ua qhov haujlwm no kom txog thaum phosphorus pentoxide (P2O5) tsis muaj xim ntxiv lawm, tom qab ntawd ntxiv cov tshiab melted anhydrous potassium carbonate (K2CO3) rau distillation kom tshem tawm cov kab ntawm phosphorus pentoxide (P2O5).
7. Ntxiv phosphorus pentoxide (5-10g/V) rau acetonitrile, reflux rau 2-3 hnub, thiab tom qab ntawd ncu nws tawm kom tshem tawm cov dej feem ntau. Nco ntsoov tias calcium chloride drying tube yuav tsum muab ntxiv rau lub raj condenser thaum lub sij hawm reflux. Kev sib ntxiv ntawm phosphorus pentoxide yuav tsum tau zam vim qhov no yuav ua rau tsim cov txiv kab ntxwv polymers. Ntxiv ib qho me me ntawm cov poov tshuaj carbonate rau cov distilled acetonitrile thiab distilled nws dua kom tshem tawm cov kab mob ntawm phosphorus pentoxide, thiab tom qab ntawd siv ib kab fractionating rau fractionation. Nws yog teeb meem heev, tab sis nws kuj yog dawb huv.
8. Ua ntej siv KMnO4 thiab K2CO3 rau reflux rau 8 teev, thiab tom qab ntawd muab tso rau hauv ib lub khob ntim hauv qab uas muaj P2O5. Reflux rau lwm 5 xuab moos thiab tom qab ntawd tawm mus.
