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p-Diiodobenzene → (z)-3-(4-Iodophenyl)-3-(4-trifluoromethylphenyl)prop-2-en-1-ol

HRID 549826
ノート
印刷プレビュー

反応式

HRID 549826 の反応式
C[O-].[Na+].[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:10][C:11]([F:23])([F:22])[C:12]1[CH:17]=[CH:16][C:15]([C:18]#[C:19][CH2:20][OH:21])=[CH:14][CH:13]=1.[I:24][C:25]1[CH:30]=[CH:29][C:28](I)=[CH:27][CH:26]=1.O1C=CC=C1P(C1OC=CC=1)C1OC=CC=1>O1CCCC1.[Cl-].[Zn+2].[Cl-].C(OCC)(=O)C>[I:24][C:25]1[CH:30]=[CH:29][C:28](/[C:18](/[C:15]2[CH:14]=[CH:13][C:12]([C:11]([F:22])([F:23])[F:10])=[CH:17][CH:16]=2)=[CH:19]\[CH2:20][OH:21])=[CH:27][CH:26]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 12208p-DiiodobenzeneHCID 521585Tris(furan-2-yl)phosphaneHCID 10942334Sodium MethoxideHCID 118304283-(4-(Trifluoromethyl)phenyl)prop-2-yn-1-olHCID 21226445Aluminium lithium hydride

生成物 1

HCID 19261707(z)-3-(4-Iodophenyl)-3-(4-trifluoromethylphenyl)prop-2-en-1-ol

試薬・触媒・溶媒

3
HCID 3007855Zincchloride触媒HCID 8028Tetrahydrofuran溶媒3 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

Sodium methoxide (12.5 mg, 0.225 mmol) was added to 1 M solution of lithium aluminum hydride in tetrahydrofuran (5 mL, 5 mmol) under argon. The mixture was cooled to 0° C. and a solution of the above alcohol (1.00 g, 5 mmol) in tetrahydrofuran (12.5 mL) was added over 10 min. The reaction was stirred at 0° C. for 3 h; dry ethyl acetate (0.825 mL) was added and the whole mixture was stirred at ambient temperature for 15 min. A degassed solution of 1,4-diiodobenzene (2.15 g, 6.5 mmol) in dry tetrahydrofuran (5 mL), anhydrous zinc chloride (0.408 g, 3 mmol), tris(dibenzylideneacetone)dipalladium chloroform complex (0.103 g, 0.1 mmol), and tri(2-furyl)phosphine (92.5 mg, 0.4 mmol) were added; the mixture was degassed and then was heated at 65° C. for 15 h under nitrogen. The suspension was cooled down; methanol (2.5 mL) was added and the mixture was stirred for additional 1 h. The reaction was diluted with ether (50 mL) and saturated aqueous solution of ammonium chloride (1.25 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 (Z)-3-(4-iodophenyl)-3-(4-trifluoromethylphenyl)prop-2-en-1-ol as solidifying oil.

後処理

  1. stirringthe whole mixture was stirred at ambient temperature for 15 min
  2. customthe mixture was degassed
  3. temperaturewas heated at 65° C. for 15 h under nitrogen
  4. temperatureThe suspension was cooled down
  5. additionmethanol (2.5 mL) was added
  6. stirringthe mixture was stirred for additional 1 h
  7. additionThe reaction was diluted with ether (50 mL) and saturated aqueous solution of ammonium chloride (1.25 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)

出典と根拠

ORDレコード
ord-d54981f6131c4c30aec316e7875c7872
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943613B2

反応ノート

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