Chlorotrimethylsilane → 1-Trimethylsiloxyindene

HRID 34263

반응식

HRID 34263 반응식
[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

참가 물질

6

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 67351-IndanoneHCID 8471Triethylamine

생성물 1

HCID 140001951-Trimethylsiloxyindene

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8003Pentane용매

실험 절차

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.).

후처리

  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.)

출처 및 근거

ORD 기록
ord-4d1857117c354952a4bf1552ec242980
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04761403

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