Reaktion #460643

ord-b9465580811e4feb8cf5d726ac5575ea

Lösungsmittel

Reaktionsbedingungen

Temperatur
-50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas dropped
  2. 2
    workup.STIRRINGThe resulting mixture was stirred at the same temperature as above for two hours
  3. 3
    Sonstigeto terminate
  4. 4
    Sonstigethe reaction

Vorschrift

A solution of 22 g of hexyne in 300 ml of THF was placed in a flask, and cooled to -50° C. Then, 170 ml of a 1.55M n-hexane solution of n-butyllithium was dropped thereto. The resulting mixture was stirred at -50° C. for 15 minutes, and then a solution of 50 g of (S) 1-ethoxyethyl-N,N-dimethyllactamide as obtained in Example 1 (2) in 150 ml of THF was dropped thereto. The resulting mixture was stirred at the same temperature as above for two hours, and then an aqueous solution of 28.3 g of ammonium chloride in 200 ml of water was dropped to terminate the reaction.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05164112uspto-grants-1992_11