반응 #64705

반응 방정식

hydrochloric acid

2-methylbenzoyl chloride

methyl isocyanide

calcium carbonate

→

title compound

수율 96.6%

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

수율 96.6%

용매

acetone

water

반응 조건

후처리

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

실험 절차

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%).

출처