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Chlorotrimethylsilane → [bis(4-Fluorophenyl)](trimethylsilyloxy)(1H-1,2,4-triazol-1-ylmethyl)silan

HRID 371312
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HRID 371312 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([Si:8]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)([OH:15])[CH2:9][N:10]2[CH:14]=[N:13][CH:12]=[N:11]2)=[CH:4][CH:3]=1.Cl[Si:24]([CH3:27])([CH3:26])[CH3:25].C(N(CC)CC)C>O1CCCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([Si:8]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)([O:15][Si:24]([CH3:27])([CH3:26])[CH3:25])[CH2:9][N:10]2[CH:14]=[N:13][CH:12]=[N:11]2)=[CH:6][CH:7]=1
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HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 13474663[bis(4-fluorophenyl)]hydroxy(1H-1,2,4-triazol-1-ylmethyl)silane

생성물 1

HCID 13489949[bis(4-Fluorophenyl)](trimethylsilyloxy)(1H-1,2,4-triazol-1-ylmethyl)silan

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 1.5 g (0.0047 mol) of [bis(4-fluorophenyl)]hydroxy(1H-1,2,4-triazol-1-ylmethyl)silane in 20 ml of tetrahydrofuran was added 0.8 ml (0.0063 mol) of chlorotrimethylsilane. A solution of 0.8 ml (0.0057 mol) of triethylamine in 5 ml of tetrahydrofuran was added dropwise, giving a thick white precipitate. The mixture was stirred overnight at room temperature, then filtered and concentrated to an oil. The residue was taken up in ether, filtered, and the filtrate was evaporated to afford the title compound as a clear colorless oil: nmr (CDCl3) 0.1 (9H, s), 4.3 (2H, s), 7.2 (4H, t, J=9 Hz), 7.6 (4H, d of d, J=9,6 Hz), 8.0 (2H, s).

후처리

  1. customgiving a thick white precipitate
  2. filtrationfiltered
  3. concentrationconcentrated to an oil
  4. filtrationfiltered
  5. customthe filtrate was evaporated

출처 및 근거

ORD 기록
ord-24ace588d8c34f0a82cb240f0669cfd6
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04530922

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