Reaktion #64705

Reaktionsgleichung

hydrochloric acid

2-methylbenzoyl chloride

methyl isocyanide

calcium carbonate

→

title compound

Ausbeute 96.6%

N-methyl-2-(2-tolyl)-2-oxoacetamide

Ausbeute 96.6%

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added
2. 2
   workup.STIRRINGThe stirring of the resulting mixture
3. 3
   workup.WAITwas continued for 1 hour
4. 4
   Extraktionextracted with methylene chloride
5. 5
   WaschenThe organic layer was washed with saturated brine
6. 6
   Trocknendried over anhydrous magnesium sulfate
7. 7
   SonstigeThe solvent was evaporated under reduced pressure
8. 8
   Wascheneluted with hexane-ethyl acetate (5:1)

Vorschrift

A mixture of 2-methylbenzoyl chloride (1.55 g) and methyl isocyanide (492 mg) was stirred at 60° C. for 6 hours. Then, the mixture was diluted with acetone (20 ml), and water (4 ml) and calcium carbonate (1.00 g) were added. The stirring of the resulting mixture was continued for 1 hour. The mixture was neutralized with dilute hydrochloric acid and extracted with methylene chloride. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with hexane-ethyl acetate (5:1) to obtain the title compound (1.71 g, Yield: 96.6%).

Quelle