4-Bromo-3-fluorobenzoic acid (CAS# 153556-42-4)
Zambiri Zolozera
| Ntchito | 4-bromo-3-fluorobenzoic acid ndi mankhwala ofunika kwambiri omwe angagwiritsidwe ntchito pokonzekera mankhwala osiyanasiyana (monga anti-cancer drug benzamit). |
| Synthesis njira | 4-bromo-3-fluorobenzoic asidi akhoza analandira ndi makutidwe ndi okosijeni wa 4-bromo-3-fluorotoluene kudzera potaziyamu permanganate. (1) makutidwe ndi okosijeni: 100kg wa kg4-bromo -3-fluorotoluene, 120kg madzi ndi 0.1kg wamafuta oledzeretsa a polyether sodium sulfate (AES) amawonjezedwa motsatizana ku ketulo yopangidwa ndi galasi ya K-400L (yopangidwa ndi Jiangsu mafakitale akalowa mankhwala Equipment Co., ltd.) ndi chipangizo choyambitsa ndi kutentha ndi condensation reflux, ndiye 167kg ya potaziyamu permanganate imawonjezedwa pang'onopang'ono pansi pa kugwedezeka, kusungidwa m'malo otentha, ndikuchitapo kanthu kwa maola 9, kusiya zomwezo pambuyo pa njira ya reflux ilibenso mikanda yamafuta; (2) Sefa: sefa yankho anachita analandira sitepe (1) pamene otentha kupeza kusefera munali chandamale mankhwala 4-bromo -3-fluorobenzoic asidi; (3) Chotsani potaziyamu permanganate: Kuti muchotse potaziyamu permanganate yotsala mu kusefera, 0.1kg ya sodium sulfite iyenera kuonjezedwa ku kusefera komwe kunapezeka mu sitepe (2), kuchuluka kwa sodium sulfite kumachokera pamadzi owoneka bwino. mtundu wofiirira wa yankho. (4) acidification: mu yogwira boma, pang`onopang`ono kuwonjezera mankhwala kwa njira anapezerapo sitepe (3) ndi ndende ya 12mol/L anaikira hydrochloric acid. pamene pH mtengo wa yankho ndi 2.2, siyani kuwonjezera moyikira hydrochloric acid ndi kupitiriza anachita kwa 30min. (5) crystallization: m'malo olimbikitsa, yankho lomwe limapezeka mu sitepe (4) limakhazikika mpaka 2 ° C, ndipo makhiristo omwe amalowa mu yankho ndi 4-bromo-3-fluorobenzoic acid. Pa opareshoni, iyenera kugwedezeka mosalekeza, apo ayi 4-bromo-3-fluorobenzoic acid ipanga cholimba chachikulu, chomwe chimakhala chovuta kuthana nacho muzotsatira; (6) Kusefera ndi kuchapa: Madzi osakanikirana omwe ali ndi 4-bromo-3-fluorobenzoic acid makhiristo omwe amapezeka mu sitepe (5) ndi centrifuged kuti apeze keke ya fyuluta yomwe ndi mankhwala a 4-bromo-3-fluorobenzoic acid, mankhwala opanda pake. imatsukidwa ndi madzi oyera ndi centrifuged (pogwiritsa ntchito centrifuge yokhala ndi ntchito yotsuka) kuti iyeretsedwe. 4-bromo-3-fluorobenzoic asidi; (7) Kuyanika: The 4-bromo-3-fluorobenzoic acid yolimba yokonzedwa mu sitepe (6) imawuma pa 75 ° C kwa maola 12 kuti ipeze 197 kg4-bromo-3-fluorobenzoic acid, yomwe ili yaikulu kuposa 98 %. |
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