Imidazole → 7-Chloro-4-methyl-4-trimethylsilyloxy-1-heptyne

HRID 126704ノート

反応式

HRID 126704 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([OH:10])([CH3:9])[CH2:6][C:7]#[CH:8].CN(C)C=O.N1C=CN=C1.Cl[Si:22]([CH3:25])([CH3:24])[CH3:23]>O>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([CH3:9])([O:10][Si:22]([CH3:25])([CH3:24])[CH3:23])[CH2:6][C:7]#[CH:8]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 128987397-Chloro-4-hydroxy-4-methyl-1-heptyne

生成物 1

HCID 128987407-Chloro-4-methyl-4-trimethylsilyloxy-1-heptyne

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 7-chloro-4-hydroxy-4-methyl-1-heptyne in 80 ml. of dimethylformamide at 0° C., is added 43.8 g. (0.644 moles) of imidazole and 35.02 g. (0.322 moles of) chlorotrimethylsilane. The mixture is stirred at room temperature for 45 minutes, poured into water and extracted with hexane. The hexane solution is washed with dilute sodium bicarbonate solution, dried over magnesium sulfate and the solvent removed leaving an orange liquid. This liquid is distilled giving the desired product in the fraction boiling at 83°-88° C., 1.5 mm. as a colorless liquid.

後処理

  1. extractionextracted with hexane
  2. washThe hexane solution is washed with dilute sodium bicarbonate solution
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent removed
  5. customleaving an orange liquid
  6. distillationThis liquid is distilled

出典と根拠

ORDレコード
ord-d1e166c13c174a6c83e8b1a0087a4f0b
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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