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

HRID 750905노트

반응식

HRID 750905 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1257c62a67044f35b69da57fd762b085
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405228B2

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