Reaktion #64319

Reaktionsgleichung

6-methyl-isatoic anhydride

sodium hydride

benzyl bromide

hydrogen

→

1-benzyl-6-methyl-isatoic anhydride

Lösungsmittel

DMF

DMF

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturIt was then cooled
2. 2
   Sonstigethe solution was then evaporated under reduced pressure at 45° C
3. 3
   Sonstigethe insoluble inorganic solid was removed by filtration
4. 4
   Sonstigethe filtrate was evaporated

Vorschrift

A solution of 6-methyl-isatoic anhydride (4.5 gm) in DMF (30 ml) was added dropwise to a stirred suspension of 60% sodium hydride (1.0 gm) in DMF (20 ml) under nitrogen atmosphere. The reaction was then warmed to 45° C. and stirred until hydrogen evolution ceased. It was then cooled and a solution of benzyl bromide (4.4 gm) in DMF (10 ml) was added slowly. Stirring was continued for one hour at room temperature and the solution was then evaporated under reduced pressure at 45° C. The resulting solid was suspended in methylene chloride, the insoluble inorganic solid was removed by filtration and the filtrate was evaporated to give 1-benzyl-6-methyl-isatoic anhydride as a crystalline solid.

Quelle