Water → 2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde

HRID 603992

反応式

HRID 603992 の反応式
F[C:2]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:3]=1[CH:4]=[O:5].[CH2:14]([NH:18][CH2:19][CH3:20])[CH2:15][CH2:16][CH3:17].C(=O)([O-])[O-].[K+].[K+].O>C1(C)C=CC=CC=1.C(OCC)C>[CH2:14]([N:18]([CH2:19][CH3:20])[C:2]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:3]=1[CH:4]=[O:5])[CH2:15][CH2:16][CH3:17]

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 25914ButylethylamineHCID 27349042-Fluoro-5-(trifluoromethyl)benzaldehyde

生成物 1

HCID 866267522-(Butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde収率 91.9%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

実験手順

2-Fluoro-5-trifluoromethyl-benzaldehyde (5.0 g) and butyl-ethyl-amine (3.95 g) are dissolved in toluene (50 ml) and thereto is added potassium carbonate (10.78 g) and the mixture is heated under reflux overnight. The reaction solution is cooled to room temperature, and thereto are added water and diethyl ether, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=19:1→4:1) to give 2-(butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde (6.54 g). MS (m/z): 274 [M+H]+

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux overnight
  3. customthe mixture is separated
  4. washthe organic layer is washed with a saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=19:1→4:1)

出典と根拠

ORDレコード
ord-8797808e003843358f9208d04ccbea49
出典データセット
uspto-grants-2011_03
特許番号
US07906517B2

関連ノート

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