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2-(4-Bromo-2,6-dimethylphenyl)-3-methoxy-cyclopent-2-enone → 2-(2,6-Dimethyl-4-prop-1-ynylphenyl)-3-methoxycyclopent-2-enone

HRID 514191
ノート
印刷プレビュー

反応式

HRID 514191 の反応式
[C:1]([Mg]Br)#[C:2][CH3:3].Br[C:7]1[CH:12]=[C:11]([CH3:13])[C:10]([C:14]2[C:15](=[O:21])[CH2:16][CH2:17][C:18]=2[O:19][CH3:20])=[C:9]([CH3:22])[CH:8]=1>O1CCCC1.[Br-].[Zn+2].[Br-].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH3:3][C:2]1[CH:1]=[C:7]([C:12]#[C:11][CH3:13])[CH:8]=[C:9]([CH3:22])[C:10]=1[C:14]1[C:15](=[O:21])[CH2:16][CH2:17][C:18]=1[O:19][CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 668681542-(4-Bromo-2,6-dimethylphenyl)-3-methoxy-cyclopent-2-enoneHCID 178419101HCID 178419101、化合物

生成物 1

HCID 896009282-(2,6-Dimethyl-4-prop-1-ynylphenyl)-3-methoxycyclopent-2-enone

試薬・触媒・溶媒 3

HCID 10421208Zinc bromide触媒HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of anhydrous zinc bromide (1.41 g, 6.3 mmol) in anhydrous tetrahydrofuran (8.0 ml) under nitrogen at 0°C., is added propynylmagnesium bromide (15.7 ml, 6.3 mmol, 0.4 M solution in tetrahydrofuran) dropwise. The reaction mixture is then allowed to warm to room temperature and stir for 10 minutes, then cooled again to 0°C. To this mixture is then added [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.102 g, 0.13 mmol), followed by a solution of 2-(4-bromo-2,6-dimethylphenyl)-3-methoxycyclopent-2-enone (0.370 g, 1.25 mmol) in anhydrous tetrahydrofuran (4.0 ml). The reaction mixture is heated at reflux for 4.5 hours, then allowed to cool to room temperature followed by quenching with saturated aqueous ammonium chloride (10 ml). Ethyl acetate is added, and the mixture is filtered through a bed of diatomaceous earth and the phases separated. The aqueous phase is extracted again with ethyl acetate (×3) and combined organics are washed with brine, dried over magnesium sulfate, filtered and the filtrate concentrated in vacuo. The residue is purified by flash column chromatography (ethyl acetate and isohexane as eluant) to afford 2-(2,6-dimethyl-4-prop-1-ynylphenyl)-3-methoxycyclopent-2-enone.

後処理

  1. temperaturecooled again to 0°C
  2. temperatureThe reaction mixture is heated
  3. temperatureat reflux for 4.5 hours
  4. temperatureto cool to room temperature
  5. customby quenching with saturated aqueous ammonium chloride (10 ml)
  6. additionEthyl acetate is added
  7. filtrationthe mixture is filtered through a bed of diatomaceous earth
  8. customthe phases separated
  9. extractionThe aqueous phase is extracted again with ethyl acetate (×3)
  10. washcombined organics are washed with brine
  11. dry with materialdried over magnesium sulfate
  12. filtrationfiltered
  13. concentrationthe filtrate concentrated in vacuo
  14. customThe residue is purified by flash column chromatography (ethyl acetate and isohexane as eluant)

出典と根拠

ORDレコード
ord-5bd59fc45cb84060ad2314942be37297
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09107415B2

反応ノート

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