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

HRID 36429

反応式

HRID 36429 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 11780091N-methyl-2-(2-phenoxyphenyl)-2-oxoacetamide収率 87.1%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-9a96245cefaa4e4aac5f8161d0bf5ca1
出典データセット
uspto-grants-1995_05
特許番号
US05414122

関連ノート

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