354-08-5Relevant articles and documents
Continuous Process for Preparing the Difluoromethylating Reagent [(DMPU)2Zn(CF2H)2] and Improved Synthesis of the ICHF2Precursor
Monfette, Sebastien,Fang, Yuan-Qing,Bio, Matthew M.,Brown, Adam R.,Crouch, Ian T.,Desrosiers, Jean-Nicolas,Duan, Shengquan,Hawkins, Joel M.,Hayward, Cheryl M.,Peperni, Nikita,Rainville, Joseph P.
, p. 1077 - 1083 (2020/05/19)
Complex [(DMPU)2Zn(CF2H)2] 1 is a crystalline organometallic reagent with utility in various catalytic difluoromethylation reactions under mild conditions. Unfortunately, this reagent is not commercially available and the procedure for the preparation of this air- and moisture-sensitive zinc complex has only been reported on a small scale. Herein, we report the development of a continuous process for the preparation of reagent 1 on >100 g scale by using a continuous stirred-tank reactor. The key to success is the design of a continuous reactive crystallization process in which the precipitation of the zinc complex 1 is driven by its low solubility in the reaction solvent. The improved synthesis of the iododifluoromethane precursor 2 from readily available bromodifluoroacetic acid further enables the synthesis of complex 1 on a larger scale.
REACTIONS OF PERHALOCARBONS. PART IX. CONVERSION OF PER(POLY)FLUOROALKYL HALIDES INTO THE CORRESPONDING CARBOCYCLIC ACIDS WITH A REDOX SYSTEM
Hu, Chang-Ming,Qing, Feng-Ling,Zhang, Hong-Gen
, p. 275 - 280 (2007/10/02)
The conversion of per(poly)fluoroalkylhalides into the corresponding carbocyclic acids with a redox system-(NH4)2S2O8/HCO2Na is described.The reaction provides a convenient method for the synthesis of various per(poly)fluorocarboxylic acids under mild conditions.