90-91-5Relevant articles and documents
Method for continuously preparing thiamphenicol by using micro-reaction system
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Paragraph 0021-0043, (2021/08/14)
The invention belongs to the technical field of pharmaceutical engineering, and particularly relates to a method for continuously preparing thiamphenicol by using a micro-reaction system. A micro-reaction system used in the method comprises a micro-mixer, a micro-channel reactor and a back pressure device, and during preparation, a solution of raw materials (1R,2R)-2-amino-1-(4-(methylsulfonyl)phenyl)propane-1,3-diol and an alkaline solution of methyl dichloroacetate are simultaneously injected into the micro-reactor by a pump respectively for condensation reaction, and concentrating, recrystallizing, filtering, washing and drying are conducted on the reaction product to obtain a thiamphenicol product. According to the method provided by the invention, the reaction time is only several minutes, the yield of the product thiamphenicol is greater than 99%, the purity is greater than 99%, the operation is convenient, continuous and controllable, the amplification effect is avoided, the efficiency of the technological process is high, and the method has a very good industrial application prospect.
Unified Strategy to Amphenicol Antibiotics: Asymmetric Synthesis of (-)-Chloramphenicol, (-)-Azidamphenicol, and (+)-Thiamphenicol and Its (+)-3-Floride
Liu, Jinxin,Li, Yaling,Ke, Miaolin,Liu, Minjie,Zhan, Pingping,Xiao, You-Cai,Chen, Fener
, p. 15360 - 15367 (2020/11/30)
The asymmetric synthesis of (-)-chloramphenicol, (-)-azidamphenicol, and (+)-thiamphenicol and its (+)-3-floride, (+)-florfenicol, is reported. This approach toward the amphenicol antibiotic family features two key steps: (1) a cinchona alkaloid derived urea-catalyzed aldol reaction allows highly enantioselective access to oxazolidinone gem-diesters and (2) a continuous flow diastereoselective decarboxylation of thermally stable oxazolidinone gem-diesters to form the desired trans-oxazolidinone monoesters with two adjacent stereocenters that provide the desired privileged scaffolds of syn-vicinal amino alcohols in the amphenicol family.
Florfenicol intermediate synthesis method
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, (2019/07/04)
The invention belongs to the field of synthesis of pharmaceutical raw materials, and specifically discloses a florfenicol intermediate synthesis method, which comprises: (1) carrying out a reaction ona compound (II) and an acylating reagent in an organic solvent to form a compound (III); (2) carrying out a reaction on the compound (III) and an oxidizing agent in an organic solvent in the presenceof a catalyst to form a compound (IV); (3) carrying out a reaction on the compound (IV) and a fluorinating reagent in an organic solvent to form a compound (V); and (4) carrying out acidolysis on thecompound (V) in an organic solvent, and carrying out deprotection to obtain a compound (I), wherein various groups in the formulas are defined in the specification. According to the present invention, the florfenicol intermediate can be used for preparing florfenicol; and the method has characteristics of novel design, mild conditions and simple operation, and is suitable for industrial production.