Chlorotrimethylsilane → 1-Trimethylsiloxyindene

HRID 34263

反応式

HRID 34263 の反応式
[CH3:1][Si:2](Cl)([CH3:4])[CH3:3].C(N(CC)CC)C.[C:13]1(=[O:22])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:15][CH2:14]1>CN(C)C=O.CCCCC>[CH3:1][Si:2]([CH3:4])([CH3:3])[O:22][CH:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14]1

参加物

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 67351-IndanoneHCID 8471Triethylamine

生成物 1

HCID 140001951-Trimethylsiloxyindene

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8003Pentane溶媒

実験手順

Trimethylsilyl chloride (5.7 g, 52.3 mmole), triethylamine (11.71 g, 116 mmole), and 1-indanone (6.22 g, 47.1 mmole) were dissolved in dimethyl formamide (25 mL) and refluxed for 17 hours. After cooling, the mixture was diluted with pentane (50 mL) and washed four times with saturated sodium bicarbonate. After backwashing the aqueous phase with pentane the organic layers were combined, washed with cold 2N HCl and cold saturated sodium bicarbonate, then dried over MgSO4. The solvent was evaporated and the residue distilled (bp 123°-125° C.).

後処理

  1. temperaturerefluxed for 17 hours
  2. temperatureAfter cooling
  3. washwashed four times with saturated sodium bicarbonate
  4. washwashed with cold 2N HCl and cold saturated sodium bicarbonate
  5. dry with materialdried over MgSO4
  6. customThe solvent was evaporated
  7. distillationthe residue distilled (bp 123°-125° C.)

出典と根拠

ORDレコード
ord-4d1857117c354952a4bf1552ec242980
出典データセット
uspto-grants-1988_08
特許番号
US04761403

関連ノート

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