反応 #64705

反応方程式

hydrochloric acid

2-methylbenzoyl chloride

methyl isocyanide

calcium carbonate

→

title compound

収率 96.6%

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

収率 96.6%

溶媒

acetone

water

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.STIRRINGThe stirring of the resulting mixture
3. 3
   workup.WAITwas continued for 1 hour
4. 4
   抽出extracted with methylene chloride
5. 5
   洗浄The organic layer was washed with saturated brine
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   その他The solvent was evaporated under reduced pressure
8. 8
   洗浄eluted with hexane-ethyl acetate (5:1)

実験手順

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%).

出典