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

HRID 603992

반응식

HRID 603992 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

실험 절차

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]+

후처리

  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)

출처 및 근거

ORD 기록
ord-8797808e003843358f9208d04ccbea49
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906517B2

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