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

HRID 126741ノート

反応式

HRID 126741 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. additiondiluted with 350 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-ab0a8fa85001482a928e673cd9855bea
出典データセット
uspto-grants-1981_03
特許番号
US04254036

反応ノート

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