Reaktion #50653
ord-748add2775f04e51ab3cbf51a8fb0c41
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONis added in small fractions
- 2workup.ADDITIONAt the end of the addition
- 3workup.STIRRINGthis mixture is stirred for 2 hours at 20° C
- 4SonstigeThe solvent is evaporated
- 5Sonstigethe residue is purified by chromatography on a silica column (eluant
- 6workup.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%).