Chlorotrimethylsilane → 4-(4-Trimethylsilyloxy-piperidin-1-yl)-3-fluoronitrobenzene

HRID 750905ノート

反応式

HRID 750905 の反応式
[O:1]=[C:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][C:9]=2[F:17])[CH2:4][CH2:3]1.C(N(CC)CC)C.[CH3:25][Si:26](Cl)([CH3:28])[CH3:27]>CN(C)C=O>[CH3:25][Si:26]([CH3:28])([CH3:27])[O:1][CH:2]1[CH2:3][CH2:4][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][C:9]=2[F:17])[CH2:6][CH2:7]1

参加物

5

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 37637811-(2-Fluoro-4-nitrophenyl)piperidin-4-one

生成物 1

HCID 693102754-(4-Trimethylsilyloxy-piperidin-1-yl)-3-fluoronitrobenzene収率 86%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

The mixture of 4-(4-oxo-piperidin-1-yl)-3-fluoronitrobenzene (0.250 mol), triethylamine (1.250 mol), trimethylsilylchloride (0.750 mol) in dimethylformamide was heated at 70° C. for 24 h. The solvent was removed under vacuum and to the residual mass was extracted with the ethyl acetate water mixture. The combined organic layer was dried and after removal of the solvent afforded title compound as a solid in 86% yield.

後処理

  1. customThe solvent was removed under vacuum and to the residual mass
  2. extractionwas extracted with the ethyl acetate water mixture
  3. customThe combined organic layer was dried
  4. customafter removal of the solvent

出典と根拠

ORDレコード
ord-1257c62a67044f35b69da57fd762b085
出典データセット
uspto-grants-2008_07
特許番号
US07405228B2

反応ノート

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