Imidazole → {[4-(1-Fluoroethenyl)oct-1-yn-4-yl]oxy}(trimethyl)silane

HRID 1154930ノート

反応式

HRID 1154930 の反応式
[F:1][C:2]([C:4]([OH:12])([CH2:8][CH2:9][CH2:10][CH3:11])[CH2:5][C:6]#[CH:7])=[CH2:3].N1C=CN=C1.CN(C)C=O.Cl[Si:24]([CH3:27])([CH3:26])[CH3:25]>O>[F:1][C:2]([C:4]([O:12][Si:24]([CH3:27])([CH3:26])[CH3:25])([CH2:8][CH2:9][CH2:10][CH3:11])[CH2:5][C:6]#[CH:7])=[CH2:3]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 127861924-(1-Fluoroethenyl)oct-1-yn-4-ol

生成物 1

HCID 12801788{[4-(1-Fluoroethenyl)oct-1-yn-4-yl]oxy}(trimethyl)silane

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred 0° C. solution of 13.7 g. of 4-(1-fluorovinyl)-4-hydroxy-1-octyne and 16.1 g. of imidazole in 60 ml. of anhydrous dimethylformamide is added, via a syringe over a 3 minute period, 11.6 ml. of chlorotrimethylsilane. The resulting solution is stirred at room temperature for 18 hours, cooled to 0° C., diluted with 350 ml of petroleum ether and shaken with 150 ml. of water. The organic phase is separated, washed with six 50 ml. portions of water, then 50 ml. of brine, dried over magnesium sulfate and concentrated in vacuo giving 18.9 g. of the desired product as a colorless liquid.

後処理

  1. customTo a stirred 0° C.
  2. temperaturecooled to 0° C.
  3. stirringshaken with 150 ml
  4. customThe organic phase is separated
  5. washwashed with six 50 ml
  6. dry with materialof brine, dried over magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customgiving 18.9 g

出典と根拠

ORDレコード
ord-8e69bff07d1947baa9107ae416ad0ca5
出典データセット
uspto-grants-1981_11
特許番号
US04298754

反応ノート

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