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

HRID 517175ノート

反応式

HRID 517175 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-f45bb5638b39415988f1d003208cf4c6
出典データセット
uspto-grants-2015_08
特許番号
US09115093B2

反応ノート

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