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Ethyl Acetate → (e)-3-(4-Iodophenyl)-3-(3-trifluoromethylphenyl)prop-2-en-1-ol

HRID 1810658
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HRID 1810658 반응식
C[O-].[Na+].[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:10][C:11]([F:23])([F:22])[C:12]1[CH:13]=[C:14]([C:18]#[C:19][CH2:20][OH:21])[CH:15]=[CH:16][CH:17]=1.C(OCC)(=O)C.[I:30][C:31]1[CH:36]=[CH:35][C:34](I)=[CH:33][CH:32]=1.O1C=CC=C1P(C1OC=CC=1)C1OC=CC=1>O1CCCC1.[Cl-].[Zn+2].[Cl-]>[I:30][C:31]1[CH:36]=[CH:35][C:34](/[C:18](/[C:14]2[CH:15]=[CH:16][CH:17]=[C:12]([C:11]([F:22])([F:23])[F:10])[CH:13]=2)=[CH:19]\[CH2:20][OH:21])=[CH:33][CH:32]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 8857Ethyl AcetateHCID 12208p-DiiodobenzeneHCID 521585Tris(furan-2-yl)phosphaneHCID 10942334Sodium MethoxideHCID 21226445Aluminium lithium hydrideHCID 227309473-(3-(Trifluoromethyl)phenyl)prop-2-yn-1-ol

생성물 1

HCID 19261273
(e)-3-(4-Iodophenyl)-3-(3-trifluoromethylphenyl)prop-2-en-1-ol

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 8028Tetrahydrofuran용매3회

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온도
0 °C

실험 절차

Sodium methoxide (90 mg, 1.67 mmol) was added to 1 M solution of lithium aluminum hydride in tetrahydrofuran (33 mL, 33 mmol) under argon. The mixture was cooled to 0° C. and a solution of the above alcohol (6.7 g, 33.5 mmol) in tetrahydrofuran (25 mL) was added over 10 min. The reaction was stirred at 0° C. for 3 h; dry ethyl acetate (10 mL, 103 mmol) was added and the whole mixture was stirred at ambient temperature for 15 min. A degassed solution of 1,4-diiodobenzene (13.25 g, 40.1 mmol) in dry tetrahydrofuran (25 mL), anhydrous zinc chloride (2.73 g, 20.0 mmol), tris(dibenzylideneacetone)dipalladium chloroform complex (0.692 g, 0.66 mmol), and tri(2-furyl)phosphine (0.854 g, 3.6 mmol) were added; the mixture was degassed and then was heated at 60° C. for 15 h under argon. The suspension was cooled down; methanol (16 mL) was added and the mixture was stirred for additional 1 h. The reaction was diluted with ether (350 mL) and saturated aqueous solution of ammonium chloride (9 mL) was added. The mixture was filtered through a paddle of silica gel and the paddle was thoroughly washed with ether (100 mL). The solvents were evaporated in vacuo and the residue was purified by flash column chromatography (silica gel Fluka 60, hexanes/ethyl acetate 5:1) affording (E)-3-(4-iodophenyl)-3-(3-trifluoromethylphenyl)prop-2-en-1-ol as solidifying oil.

후처리

  1. stirringthe whole mixture was stirred at ambient temperature for 15 min
  2. customthe mixture was degassed
  3. temperaturewas heated at 60° C. for 15 h under argon
  4. temperatureThe suspension was cooled down
  5. additionmethanol (16 mL) was added
  6. stirringthe mixture was stirred for additional 1 h
  7. additionThe reaction was diluted with ether (350 mL) and saturated aqueous solution of ammonium chloride (9 mL)
  8. additionwas added
  9. filtrationThe mixture was filtered through a paddle of silica gel
  10. washthe paddle was thoroughly washed with ether (100 mL)
  11. customThe solvents were evaporated in vacuo
  12. customthe residue was purified by flash column chromatography (silica gel Fluka 60, hexanes/ethyl acetate 5:1)

출처 및 근거

ORD 기록
ord-e5cb8dfb730e42df891e6d98c35f75ed
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362016B2

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