Reaktion #56153

ord-88eb27fe145143528c64dd0096180b8c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGStirring
  2. 2
    ExtraktionThe equilibrated aqueous phase is then extracted with two 100 ml
  3. 3
    WaschenThe combined organic phase is then washed twice with approximately 100 ml

Vorschrift

To 41.4 g. (0.1 mole) of 1,3-bis-iodomethyl-1,1,3,3-tetramethyl-disiloxane there is added dropwise with stirring 32.4 g. (0.3 mole) of 2-aminomethyl-pyridine while maintaining the temperature at 20° C. Stirring is continued at room temperature for 24 hours. The now heterogeneous mixture is combined with approximately 0.5 l. of toluene followed by approximately 0.5 l. of water. The equilibrated aqueous phase is then extracted with two 100 ml. portions of toluene. The combined organic phase is then washed twice with approximately 100 ml. of water to give 4-(2-pyridylmethyl)-2,2,6,6-tetramethyl-1-oxa-4-aza-2,6-disilacyclohexane as the crude free base.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04224317uspto-grants-1980_09