Reaktion #50653

ord-748add2775f04e51ab3cbf51a8fb0c41

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONis added in small fractions
  2. 2
    workup.ADDITIONAt the end of the addition
  3. 3
    workup.STIRRINGthis mixture is stirred for 2 hours at 20° C
  4. 4
    SonstigeThe solvent is evaporated
  5. 5
    Sonstigethe residue is purified by chromatography on a silica column (eluant
  6. 6
    workup.ADDITIONa mixture of dichloromethane, 40% and hexane, 60%)

Vorschrift

The compound obtained above in part (a), (30.85 g, 90 mmoles), is dissolved in 100 ml of dry THF and then treated with 2.7 g (90 mmoles) of sodium hydride (80% in oil) which is added in small fractions. At the end of the addition, the mixture is stirred for 30 minutes at ambient temperature. 12.8 g (90 mmole) of methyl iodide are then added and this mixture is stirred for 2 hours at 20° C. The solvent is evaporated and the residue is purified by chromatography on a silica column (eluant: a mixture of dichloromethane, 40% and hexane, 60%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05428052uspto-grants-1995_06