I-4-Bromo-3-fluorobenzoic acid (CAS# 153556-42-4)
Ulwazi lweReference
Usebenzisa | I-4-bromo-3-fluorobenzoic acid yinto ebalulekileyo yekhemikhali ekrwada engasetyenziselwa ukulungiselela iintlobo ezahlukeneyo zeziyobisi (ezifana ne-anti-cancer drug benzamit). |
Indlela yokudibanisa | I-4-bromo-3-fluorobenzoic acid inokufumaneka nge-oxidation ye-4-bromo-3-fluorotoluene nge-potassium permanganate. (1) i-oxidation: i-100kg ye-kg4-bromo -3-fluorotoluene, i-120kg yamanzi kunye ne-0.1kg ye-alcohol enamafutha e-polyether sodium sulfate (AES) yongezwa ngokulandelelana kwi-kettle ye-K-400L ye-glass-lined reaction (eyenziwe yi-Jiangsu industrial lining chemicals). izixhobo co., ltd.) ngokushukumisa kunye nokufudumeza kunye nesixhobo reflux condensation, ngoko I-167kg ye-potassium permanganate yongezwa ngokucothayo phantsi kwemeko evuselelayo, igcinwe kwindawo ebilayo, kwaye iphendule iiyure ezili-9, yeka ukusabela emva kokuba isisombululo se-reflux singasenawo amaso e-oyile; 2 (3) Susa i-potassium permanganate: Ukuze kususwe i-potassium permanganate eseleyo kwi-filtrate, i-0.1kg ye-sodium sulfite kufuneka ifakwe kwi-filtrate efunyenwe kwinqanaba (2), isixa esongezelelweyo se-sodium sulfite sisekelwe kulwelo olucacileyo kunye umbala omfusa wesisombululo. (4) i-acidification: kwisimo esichukumisayo, ngokukhawuleza yongeza i-substance kwisisombululo esifunyenwe kwisinyathelo (3) kunye noxinzelelo lwe-12mol / L concentrated hydrochloric acid. xa ixabiso le-pH lesisombululo li-2.2, yeka ukongeza i-hydrochloric acid egxininisiweyo kwaye uqhubeke nokusabela kwi-30min. (5) i-crystallization: kwimeko ephazamisayo, isisombululo esifunyenwe kwisinyathelo (4) sipholile ukuya kwi-2 ° C, kunye ne-crystals ehlanjululwe kwisisombululo yi-4-bromo-3-fluorobenzoic acid. Ngethuba lokusebenza, kufuneka iqhutywe ngokuqhubekayo, ngaphandle koko i-4-bromo-3-fluorobenzoic acid iya kwenza i-slide enkulu, okunzima ukujongana nayo kwiinkqubo ezilandelayo; (6) Ukuhluzwa kunye nokuhlamba: Ulwelo oluxutyiweyo oluqulathe iikristale zeasidi ezi-4-bromo-3-fluorobenzoic ezifunyenwe kwinyathelo (5) lugxininiswe ukuze kufumaneke ikeyiki yokucoca eyimveliso yeasidi eyi-4-bromo-3-fluorobenzoic ekrwada, imveliso ekrwada. ihlanjwe ngamanzi acocekileyo kunye ne-centrifuged (usebenzisa i-centrifuge enomsebenzi wokuvasa) ukufumana ephuculweyo. 4-bromo-3-fluorobenzoic acid; (7) Ukomisa: I-4-bromo-3-fluorobenzoic acid eqinileyo elungiselelwe kwinqanaba (6) yomiswe kwi-75 ° C kwiiyure ze-12 ukufumana i-197 kg4-bromo-3-fluorobenzoic acid, umxholo wayo ungaphezulu kwe-98 %. |
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