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...
Gespeichert in:
Hauptverfasser: | , , , , , |
---|---|
Format: | Patent |
Sprache: | chi ; eng |
Schlagworte: | |
Online-Zugang: | Volltext bestellen |
Tags: |
Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
|
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 |
---|