4-Bromo-3-fluorobenzoic acid (CAS# 153556-42-4)
Reference Information
| Uses | 4-bromo-3-fluorobenzoic acid inokosha kemikari yakasvibiswa inogona kushandiswa kugadzira mishonga yakasiyana-siyana (yakadai se-anti-cancer drug benzamit). |
| Synthesis nzira | 4-bromo-3-fluorobenzoic acid inogona kuwanikwa ne oxidation ye 4-bromo-3-fluorotoluene kuburikidza ne potassium permanganate. (1) oxidation: 100kg yekg4-bromo -3-fluorotoluene, 120kg yemvura uye 0.1kg yemafuta edoro polyether sodium sulfate (AES) inowedzerwa sequentially kuK-400L girazi-lined reaction kettle (yakagadzirwa neJiangsu industrial lining chemikemikari. midziyo co., ltd.) ine inomutsa uye kudziyisa uye condensation reflux mudziyo, ipapo 167kg ye potassium permanganate inowedzerwa zvishoma nezvishoma pasi pemamiriro ekusimudzira, inochengetwa mumamiriro ekuvira, uye inogadzirisa kwemaawa mapfumbamwe, misa maitiro mushure mokunge mushonga we reflux usisina mafuta emafuta; (2) Filtration: sefa mhinduro mhinduro inowanikwa munhanho (1) ichipisa kuwana filtrate ine chinangwa chigadzirwa 4-bromo -3-fluorobenzoic acid; (3) Bvisa potassium permanganate: Kuti ubvise yakasara potassium permanganate mufiltrate, 0.1kg yesodium sulfite inofanirwa kuwedzerwa kune filtrate inowanikwa mudanho (2), iyo yekuwedzera yesodium sulfite yakavakirwa pamvura inoonekera ine. ruvara rwepepuru rwemhinduro. (4) acidification: mumamiriro ekukurudzira, zvishoma nezvishoma wedzera chinhu kumushonga unowanikwa munhanho (3) nehuwandu hwe12mol / L concentrated hydrochloric acid. kana iyo pH kukosha kwemhinduro iri 2.2, mira kuwedzera concentrated hydrochloric acid uye enderera mberi nekuita kwe30min. (5) crystallization: mumamiriro ezvinhu anokurudzira, mhinduro inowanikwa munhanho (4) inotonhorera kusvika ku2 ° C, uye makristasi anonaya mumushonga ndeye 4-bromo-3-fluorobenzoic acid. Panguva yekushanda, inofanira kusimudzwa nguva dzose, kana zvisina kudaro 4-bromo-3-fluorobenzoic acid ichaita yakasimba yakasimba, iyo yakaoma kubata nayo mune zvinotevera; (6) Kusefeta nekugezwa: Mvura yakasanganiswa ine 4-bromo-3-fluorobenzoic acid makristasi inowanikwa mudanho (5) inoiswa mukati kuti iwane keke resefa iro riine crude 4-bromo-3-fluorobenzoic acid chigadzirwa, crude chigadzirwa. inoshambidzwa nemvura yakachena uye centrifuged (uchishandisa centrifuge ine washing basa) kuwana yakanatswa. 4-bromo-3-fluorobenzoic asidhi; (7) Kuomesa: Iyo 4-bromo-3-fluorobenzoic asidhi yakasimba yakagadzirwa mudanho (6) inoomeswa pa 75 ° C kwemaawa gumi nemaviri kuti iwane 197 kg4-bromo-3-fluorobenzoic acid, iyo inodarika 98 %. |
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