Imidazole → Hexaethyldisiloxane

HRID 481802ノート

反応式

HRID 481802 の反応式
N1[CH:5]=[CH:4]N=C1.[CH2:6]([Si:8](Cl)([CH2:11][CH3:12])[CH2:9][CH3:10])[CH3:7].[OH2:14]>CN(C)C=O>[CH2:6]([Si:8]([O:14][Si:8]([CH2:4][CH3:5])([CH2:9][CH3:10])[CH2:6][CH3:7])([CH2:11][CH3:12])[CH2:9][CH3:10])[CH3:7]

参加物

5

反応物 3

HCID 795ImidazoleHCID 962WaterHCID 13819Chlorotriethylsilane

生成物 1

HCID 70442Hexaethyldisiloxane

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 205 (15 mmol) in dimethylformamide (30 mL) is cooled to 0° C. and treated with imidazole (30 mmol) and triethylsilyl chloride (20 mmol). The resultant solution is warmed to room temperature. After 12 h, the reaction mixture is poured into 300 mL of water and extracted with ether (3×40 mL). The ethereal extracts are washed with water (2×25 mL) and saturated aqueous brine (25 mL), dried over magnesium sulfate and concentrated in vacuo. The residue is purified by flash chromatography to afford 206.

後処理

  1. extractionextracted with ether (3×40 mL)
  2. washThe ethereal extracts are washed with water (2×25 mL) and saturated aqueous brine (25 mL)
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by flash chromatography

出典と根拠

ORDレコード
ord-28682ee2c41649d19b8a2c84c6c050ec
出典データセット
uspto-grants-1998_08
特許番号
US05789605

反応ノート

読み込み中…