4-Bromo-3-fluorobenzoic acid (CAS # 153556-42-4)
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Na-eji | 4-bromo-3-fluorobenzoic acid bụ ihe dị mkpa kemịkalụ akụrụngwa nke enwere ike iji kwadebe ụdị ọgwụ dị iche iche (dịka ọgwụ mgbochi ọrịa kansa benzamit). |
Usoro synthesis | Enwere ike nweta 4-bromo-3-fluorobenzoic acid site na oxidation nke 4-bromo-3-fluorotoluene site na potassium permanganate. (1) oxidation: 100kg nke kg4-bromo -3-fluorotoluene, 120kg mmiri na 0.1kg nke mmanya na-aba n'anya polyether sodium sulfate (AES) na-agbakwunyere n'usoro nke K-400L glass-lined kettle mmeghachi omume (nke Jiangsu rụpụtara kemịkalụ ụlọ ọrụ mmepụta ihe). Equipment Co., Ltd.) na mkpali na kpo oku na condensation reflux ngwaọrụ, Mgbe ahụ, 167kg nke potassium permanganate na-eji nwayọọ nwayọọ na-agbakwunye n'okpuru ọnọdụ na-akpali akpali, na-edebe ya na steeti na-esi esi, ma meghachi omume maka awa 9, kwụsị mmeghachi omume mgbe ngwọta reflux enweghịzi mmanụ mmanụ; (2) Ntucha: nyochaa mmeghachi omume mmeghachi omume enwetara na nzọụkwụ (1) mgbe ọ na-ekpo ọkụ iji nweta nzacha nwere ihe ezubere iche 4-bromo -3-fluorobenzoic acid; (3) Wepu potassium permanganate: Iji wepụ ihe fọdụrụ potassium permanganate na filtrate, 0.1kg nke sodium sulfite ga-agbakwunyere filtrate nwetara na nzọụkwụ (2), ihe mgbakwunye ego nke sodium sulfite dabeere na mmiri mmiri na-egbuke egbuke. agba odo odo nke ngwọta. (4) acidification: na ọnọdụ na-akpali akpali, jiri nwayọọ nwayọọ tinye ihe ahụ na ngwọta enwetara na nzọụkwụ (3) na ntinye nke 12mol / L concentrated hydrochloric acid. Mgbe uru pH nke ngwọta bụ 2.2, kwụsị ịgbakwụnye hydrochloric acid ma gaa n'ihu mmeghachi omume maka 30min. (5) crystallization: na ọnọdụ na-akpali akpali, ihe ngwọta enwetara na nzọụkwụ (4) na-eme ka ọ dị mma na 2 Celsius C, na kristal na-agbanye na ngwọta bụ 4-bromo-3-fluorobenzoic acid. N'oge a na-arụ ọrụ, a ghaghị ịkpali ya na-aga n'ihu, ma ọ bụghị 4-bromo-3-fluorobenzoic acid ga-emepụta nnukwu ihe siri ike, nke siri ike ịnagide na usoro ndị na-esote; (6) Nzacha na ịsa: Mmiri mmiri agwakọta nwere 4-bromo-3-fluorobenzoic acid crystals enwetara na nzọụkwụ (5) bụ centrifuged iji nweta achicha nzacha nke bụ ngwaahịa 4-bromo-3-fluorobenzoic acid, ngwaahịa crude. a na-asa ya na mmiri dị ọcha na centrifuge (iji centrifuge nwere ọrụ ịsacha) iji nweta nụchara anụcha. 4-bromo-3-fluorobenzoic acid; (7) ihicha: 4-bromo-3-fluorobenzoic acid siri ike kwadebere na nzọụkwụ (6) na-akpọnwụ na 75 ° C maka awa 12 iji nweta 197 kg4-bromo-3-fluorobenzoic acid, ọdịnaya ya karịrị 98. % |
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