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Sodium Sulfate → 2-(5-bromo-1H-inden-2-yl)ethanol

HRID 273221
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HRID 273221 반응식
C[O:2][C:3](=O)[CH2:4][C:5]1[CH2:6][C:7]2[C:12]([CH:13]=1)=[CH:11][C:10]([Br:14])=[CH:9][CH:8]=2.[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>C(OCC)C>[Br:14][C:10]1[CH:11]=[C:12]2[C:7](=[CH:8][CH:9]=1)[CH2:6][C:5]([CH2:4][CH2:3][OH:2])=[CH:13]2
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참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 85969236methyl(5-bromo-1H-inden-2-yl)acetate

생성물 1

HCID 671042662-(5-bromo-1H-inden-2-yl)ethanol

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

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온도
0 °C

실험 절차

The product from Example 52C (1.1 g, 4.1 mmol) in diethyl ether (5 mL) was added dropwise to a suspension of lithium aluminum hydride (0.125 g, 3.3 mmol) in diethyl ether (10 mL) maintaining the internal temperature below 10° C. After stirring for 30 minutes, the reaction mixture was diluted with diethyl ether (10 mL), cooled to 0° C., and treated with saturated aqueous sodium sulfate dropwise. The ethereal solution was decanted, dried with sodium sulfate, filtered, and the filtrate was concentrated to provide the title compound which was used without further purification in the next step. 1H NMR (CDCl3) δ 2.77 (m, 2H); 3.32 (s, 2H); 3.88 (t, J=6.5 Hz, 2H); 6.56 (m, 1H), 7.23 (m, 2H); 7.40 (m, 1H).

후처리

  1. temperaturemaintaining the internal temperature below 10° C
  2. customThe ethereal solution was decanted
  3. dry with materialdried with sodium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-b75f9344878f4eda86969a0e6b98c2ba
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07456196B2

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