Reaction #362288

ord-b1bce4329ce84056b5b9556786c9c9ef

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Filtrationfiltered
  2. 2
    workup.ADDITIONmixed lithium diisopropylamide and diisobutylamide with 3% lithium tert butoxide

Procedure

1759 g (7.65 moles) of 24.2% n-butyllithium in cyclohexane is added over a 90- minute period to 3.70 diisopropylamide and 3.70 moles diisobutyl amine containing 0.3 moles tert butyl alcohol in a 5-liter three-necked flask under nitrogen. The mixture was stirred at a temperature of 20°-30° C. Butane gas evolved during the reaction through an oil by bubbler. The reaction was complete upon final addition of the butyllithium solution. The solution was polish filtered. The final product was 2.7M lithium molar mixed lithium diisopropylamide and diisobutylamide with 3% lithium tert butoxide.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05391824uspto-grants-1995_02