Method for preparing difluoroiodo-olefin

The invention belongs to the field of iodo-difluoro alkylation of alkynes and particularly relates to a method for preparing difluoroiodo-olefin. The method comprises the steps: (1) taking the alkynesas a starting raw material, adding accurate-weighed alkali into a Schlenk reaction tube with a stirr...

Ausführliche Beschreibung

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Bibliographische Detailangaben
Hauptverfasser: LI KANGKUI, ZHOU YONGYUN, CHEN JINGCHAO, SUN WEIQING, FAN RUIFENG, FAN BAOMIN
Format: Patent
Sprache:chi ; eng
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Beschreibung
Zusammenfassung:The invention belongs to the field of iodo-difluoro alkylation of alkynes and particularly relates to a method for preparing difluoroiodo-olefin. The method comprises the steps: (1) taking the alkynesas a starting raw material, adding accurate-weighed alkali into a Schlenk reaction tube with a stirrer in a glove box, plugging the Schlenk reaction tube with a rubber plug, and shifting out the Schlenk reaction tube from the glove box; (2) sucking an organic solvent with a syringe, sucking ethyl difluoro-iodoacetate and endo-yne with a trace sample injector, sequentially adding the organic solvent, the ethyl difluoro-iodoacetate and the endo-yne into the reaction tube, carrying out a stirred reaction on a constant-temperature magnetic stirrer at room temperature under the irradiation of visible light of a 30W blue LED, and monitoring a reaction process by employing TLC and GC-MS; and (3) taking out the reaction tube after the reaction ends up, removing a volatile solvent from a reactionsolution by a rotary evapo