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Tetrahydrofuran → 2-(1H-Inden-2-yl)ethan-1-ol

HRID 1071819
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HRID 1071819 반응식
ClC[SiH2][C:4]1[CH2:5][C:6]2[C:11]([CH:12]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2.C1C[O:16][CH2:15][CH2:14]1>>[CH2:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH:12]=[C:4]1[CH2:14][CH2:15][OH:16]
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참가 물질

3

반응물 2

HCID 8028Tetrahydrofuran2회HCID 131724997HCID 131724997, 화합물

생성물 1

HCID 143166262-(1H-Inden-2-yl)ethan-1-ol수율 33.4%

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온도
-78 °C

실험 절차

Under nitrogen flow, a 1 L three-necked flask receives 400 mL of THF and 8 g of 2-chloromethylsilylindene and the mixture is cooled to −78° C. To this, 38.5 mL (38.5 mmol) of a solution (1.0M) of LiN(trimethylsilylene)2 in THF is added dropwise. After stirring at room temperature for 15 hours, the solvent is distilled off and the residue is extracted with 300 mL of hexane. The solvent was distilled off to obtain 2.2 g (6.4 mmol) of (1,2′-dimethylsilylene)(2,1′-dimethylsilylene)(indene) 2 (yield: 33.4%). The results of 1H-NMR analysis (90 MHz, CDC13) are as follows: δ-0.69, 0.73 (12H, dimethylsilylene), 3.66 (4H, —CH2—), 7.17 (8H, Ar—H).

후처리

  1. distillationthe solvent is distilled off
  2. extractionthe residue is extracted with 300 mL of hexane
  3. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-dad11043b89a41b18f86249f600d1da5
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06906155B1

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