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Chlorotrimethylsilane → 3-(Trimethylsilyl)benzenemethanol

HRID 1938572
ノート
印刷プレビュー

反応式

HRID 1938572 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].C([Li])CCC.[CH3:15][Si:16](Cl)([CH3:18])[CH3:17]>C(OCC)C>[CH3:15][Si:16]([CH3:18])([CH3:17])[C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 851413-Bromobenzyl alcoholHCID 178418339Butyllithium

生成物 1

HCID 151146973-(Trimethylsilyl)benzenemethanol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of 3-bromobenzylalcohol (9.35 g, 50 mmol) in diethyl ether (50 ml) at 0° C. was added dropwise 1.5M butyllithium (66.7 ml) and the mixture was stirred 30 min. Then trimethylsilylchloride (11.39 g, 105 mmol) in diethyl ether (50 ml) was added dropwise and the mixture was stirred at room temperature 18 hours. The reaction mixture was treated with ice water (100 ml) and the organic layer extracted, washed with water, brine, dried over MgSO4 and concentrated. The crude product was dissolved in 90% aqueous methanol (100 ml) and refluxed 1 hour. The solvents were removed and 3-trimethylsilylbenzylalcohol was purified by distillation.

後処理

  1. stirringthe mixture was stirred at room temperature 18 hours
  2. extractionthe organic layer extracted
  3. washwashed with water, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. dissolutionThe crude product was dissolved in 90% aqueous methanol (100 ml)
  7. temperaturerefluxed 1 hour
  8. customThe solvents were removed
  9. distillation3-trimethylsilylbenzylalcohol was purified by distillation

出典と根拠

ORDレコード
ord-dc0edb14b0fe487489c4fc76b3432e11
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05693668

反応ノート

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