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

HRID 36429

반응식

HRID 36429 반응식
[O:1]([C:8]1[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10](Cl)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:17][N+:18]#[C-:19].C(=O)([O-])[O-:21].[Ca+2].Cl>CC(C)=O.O>[CH3:19][NH:18][C:17](=[O:21])[C:10]([C:9]1[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=1[O:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:11]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 11646Methyl isocyanideHCID 110753032-Phenoxybenzoyl chloride

생성물 1

HCID 11780091N-methyl-2-(2-phenoxyphenyl)-2-oxoacetamide수율 87.1%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

A mixture of 2-phenoxybenzoyl chloride (1.09 g) and methyl isocyanide (383 mg) was stirred at 50° C. for 3 hours. Then, the mixture was diluted with acetone (10 ml), and water (2 ml) and calcium carbonate (500 mg) were added. The resulting mixture was stirred for 1 hour. The mixture was neutralized with dilute hydrochloric acid and extracted with methylene chloride. After drying the organic layer, the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with hexane-ethyl acetate (6:1) to obtain the title compound as crystals (1.04 g, Yield: 87.1%), mp: 94°-95° C.

후처리

  1. additionwere added
  2. stirringThe resulting mixture was stirred for 1 hour
  3. extractionextracted with methylene chloride
  4. customAfter drying the organic layer
  5. customthe solvent was evaporated under reduced pressure
  6. washeluted with hexane-ethyl acetate (6:1)

출처 및 근거

ORD 기록
ord-9a96245cefaa4e4aac5f8161d0bf5ca1
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05414122

연결된 노트

불러오는 중…