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

HRID 371312
ノート
印刷プレビュー

反応式

HRID 371312 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 13474663[bis(4-fluorophenyl)]hydroxy(1H-1,2,4-triazol-1-ylmethyl)silane

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-24ace588d8c34f0a82cb240f0669cfd6
出典データセット
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04530922

反応ノート

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