Water → 4-[Ethyl(methyl)amino]benzaldehyde

HRID 1663604ノート

反応式

HRID 1663604 の反応式
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH3:10][NH:11][CH2:12][CH3:13].C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[CH2:12]([N:11]([C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1)[CH3:10])[CH3:13]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 12219N-MethylethylamineHCID 680234-Fluorobenzaldehyde

生成物 1

HCID 133962824-[Ethyl(methyl)amino]benzaldehyde収率 89%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a solution of 4-fluorobenzaldehyde (1.5 g) and methylethylamine (1.56 mL) in dimethylsulfoxide (9 mL) was added potassium carbonate (2.17 g) and the mixture was stirred by using a microwave synthesizer (Biotage LTD.) at 120° C. for 2 hours. Thereto was added water and the mixture was extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated in vacuo. The resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20) to give 4-(N-ethyl-N-methylamino)benzaldehyde (1.89 g, yield: 89%).

後処理

  1. customat 120° C.
  2. customfor 2 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20)

出典と根拠

ORDレコード
ord-5ed1b6e0df1f4b21b7ae5f6f131b099c
出典データセット
uspto-grants-2011_10
特許番号
US08034949B2

反応ノート

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