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Methyl iodide → 2-Benzyl-N-(3,5-bis-trifluoromethyl-benzyl)-N-methyl-benzamide

HRID 2186785
ノート
印刷プレビュー

反応式

HRID 2186785 の反応式
[CH2:1]([C:8]1[CH:31]=[CH:30][CH:29]=[CH:28][C:9]=1[C:10]([NH:12][CH2:13][C:14]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[C:16]([C:24]([F:27])([F:26])[F:25])[CH:15]=1)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:32][Si](C)(C)[N-][Si](C)(C)C.[K+].CI.C(OCC)(=O)C>CN(C)C=O>[CH2:1]([C:8]1[CH:31]=[CH:30][CH:29]=[CH:28][C:9]=1[C:10]([N:12]([CH2:13][C:14]1[CH:15]=[C:16]([C:24]([F:25])([F:26])[F:27])[CH:17]=[C:18]([C:20]([F:22])([F:23])[F:21])[CH:19]=1)[CH3:32])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 3251421Potassium bis(trimethylsilyl)amideHCID 98243732-Benzyl-N-(3,5-bis-trifluoromethyl-benzyl)-benzamide

生成物 1

HCID 98684212-Benzyl-N-(3,5-bis-trifluoromethyl-benzyl)-N-methyl-benzamide収率 87%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 100 mg (0.23 mmol) 2-benzyl-N-(3,5-bis-trifluoromethyl-benzyl)-benzamide in 1 ml N,N-dimethylformamide at 0° C. were added 50 mg (0.25 mmol) potassium hexamethyldisilazide. Stirring was continued for 1 h at this temperature and 0.016 ml (0.25 mmol) methyl iodide were added. After stirring for 3 h at room temperature, ethyl acetate was added. The mixture was washed with brine, dried (magnesium sulfate) and evaporated. The solvent was removed in vacuo and the residue was purified by flash chromatography to give 90 mg (87%) of the title compound as a colourless oil.

後処理

  1. additionwere added
  2. stirringAfter stirring for 3 h at room temperature
  3. washThe mixture was washed with brine
  4. dry with materialdried (magnesium sulfate)
  5. customevaporated
  6. customThe solvent was removed in vacuo
  7. customthe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-06075aa6fa864525aa5621d3f988052f
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06407111B1

反応ノート

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