Imidazole → 4-Trimethylsilylethynyl-1-octyn-4-ol trimethylsilyl ether

HRID 126725ノート

反応式

HRID 126725 の反応式
[CH3:1][Si:2]([C:5]#[C:6][C:7]([OH:15])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:8][C:9]#[CH:10])([CH3:4])[CH3:3].N1C=CN=C1.CN(C)C=O.Cl[Si:27]([CH3:30])([CH3:29])[CH3:28]>CCCCCC>[CH3:28][Si:27]([O:15][C:7]([C:6]#[C:5][Si:2]([CH3:3])([CH3:1])[CH3:4])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:8][C:9]#[CH:10])([CH3:30])[CH3:29]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 127861934-Trimethylsilylethynyl-1-octyn-4-ol

生成物 1

HCID 572330774-Trimethylsilylethynyl-1-octyn-4-ol trimethylsilyl ether

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

To a stirred mixture of 8.5 g. of 4-trimethylsilylethynyl-1-octyn-4-ol and 6.2 g. of imidazole in 24 ml. of dry dimethylformamide is added, under nitrogen, 5.7 ml. of chlorotrimethylsilane, in a slow stream, via a syringe. The mixture is stirred in an ice-bath for one hour and then at room temperature overnight. The mixture is poured into hexane, washed with saturated sodium bicarbonate solution, water and then brine and dried over sodium sulfate. The solvents are evaporated to dryness giving 11.1 g. of the desired product.

後処理

  1. additionTo a stirred mixture of 8.5 g
  2. customat room temperature
  3. customovernight
  4. washwashed with saturated sodium bicarbonate solution, water
  5. dry with materialbrine and dried over sodium sulfate
  6. customThe solvents are evaporated to dryness
  7. customgiving 11.1 g

出典と根拠

ORDレコード
ord-868cba1401de44109d9bfa28ba80cd9f
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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