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Aluminium lithium hydride → HCID 53275778, 화합물

HRID 889021
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HRID 889021 반응식
C([O:3][C:4]([CH:6]1[CH2:8][CH:7]1[C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[F:16][C:15]([F:17])([F:18])[C:11]1[CH:10]=[C:9]([CH:7]2[CH2:8][CH:6]2[CH2:4][OH:3])[CH:14]=[CH:13][CH:12]=1
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참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 574296592-(3-Trifluoromethyl-phenyl)-cyclopropanecarboxylic acid ethyl ester

생성물 1

HCID 53275778HCID 53275778, 화합물수율 92.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
22.5 °C

실험 절차

2-(3-Trifluoromethyl-phenyl)-cyclopropanecarboxylic acid ethyl ester (prepared as per literature procedure) (0.70 g, 2.7 mmol) in THF (5 ml) was added to a solution of lithium aluminium hydride (0.123 g, 3.25 mmol) in THF (5 ml) at 0° C. over a period of 10 min. and stirred further at 20-25° C. for 2 hours. The reaction mixture was diluted with THF (15 ml) and quenched with 10% NaOH solution (5 ml) and water (10 ml). The aqueous layer was extracted with ethyl acetate, washed with saturated brine solution and dried over Na2SO4. The organic layer was evaporated to afford [2-(3-trifluoromethyl-phenyl)-cyclopropyl]-methanol as a colorless oil (0.54 g, 92%).

후처리

  1. customquenched with 10% NaOH solution (5 ml) and water (10 ml)
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. washwashed with saturated brine solution
  4. dry with materialdried over Na2SO4
  5. customThe organic layer was evaporated

출처 및 근거

ORD 기록
ord-503da88fceca4934aee6d04ca9cbcd49
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252797B2

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