Hydrochloric Acid → N-methyl-2-(2-methylphenyl)-2-oxoacetamide

HRID 36427

반응식

HRID 36427 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH3:11][N+:12]#[C-:13].C(=O)([O-])[O-:15].[Ca+2].Cl>CC(C)=O.O>[CH3:13][NH:12][C:11](=[O:15])[C:4]([C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=1[CH3:1])=[O:5]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 11646Methyl isocyanideHCID 702762-Methylbenzoyl chloride

생성물 1

HCID 15239356N-methyl-2-(2-methylphenyl)-2-oxoacetamide수율 96.6%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

반응 조건

온도
60 °C

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%).

후처리

  1. additionwere added
  2. stirringThe stirring of the resulting mixture
  3. waitwas continued for 1 hour
  4. extractionextracted with methylene chloride
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. washeluted with hexane-ethyl acetate (5:1)

출처 및 근거

ORD 기록
ord-336b3b8c2eb143d68f7aa0398be0a69a
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05414122

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