Dimethylformamide → 6,6-Dimethyl-3-(3-(trifluoromethyl)phenylamino)cyclohex-2-enone

HRID 517175노트

반응식

HRID 517175 반응식
[CH3:1][C:2]1([CH3:10])[CH2:7][CH2:6][C:5](=O)[CH2:4][C:3]1=[O:9].[F:11][C:12]([F:21])([F:20])[C:13]1[CH:14]=[C:15]([CH:17]=[CH:18][CH:19]=1)[NH2:16].FC(F)(F)S([O-])(=O)=O.[Yb+3].FC(F)(F)S([O-])(=O)=O.FC(F)(F)S([O-])(=O)=O.CN(C)C=O>O.CO>[CH3:1][C:2]1([CH3:10])[C:3](=[O:9])[CH:4]=[C:5]([NH:16][C:15]2[CH:17]=[CH:18][CH:19]=[C:13]([C:12]([F:11])([F:20])[F:21])[CH:14]=2)[CH2:6][CH2:7]1

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 73753-(Trifluoromethyl)anilineHCID 1363601,3-Cyclohexanedione, 4,4-dimethyl-HCID 2733225Ytterbium triflate

생성물 1

HCID 867322966,6-Dimethyl-3-(3-(trifluoromethyl)phenylamino)cyclohex-2-enone

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A mixture of 4,4-dimethylcyclohexane-1,3-dione (563 mg, 4.02 mmol), 3-(trifluoromethyl)aniline (500 μL, 645 mg, 4.02 mmol), Ytterbium(III) trifluormethanesulfonate (12.5 mg, 20 μmol, 0.5 mol %) and N,N-dimethylformamide (2.5 mL) is stirred at room temperature over night. Methanol and water are added and the mixture is filtered. The precipitate is washed with water and dried under reduced pressure. Yield: 654 mg; ESI mass spectrum [M+H]+=284, Retention time HPLC: 1.18 min (Z005—001).

후처리

  1. filtrationthe mixture is filtered
  2. washThe precipitate is washed with water
  3. customdried under reduced pressure
  4. custom1.18 min (Z005—001)

출처 및 근거

ORD 기록
ord-f45bb5638b39415988f1d003208cf4c6
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115093B2

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