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Pyridine → 2-(2-BROMO-5-METHOXYPHENYL)ETHANOL

HRID 1978896
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1978896
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[CH2:6][CH2:7][OH:8].N1C=CC=CC=1.[Br:18]Br>ClCCl>[Br:18][C:9]1[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[CH:4][C:5]=1[CH2:6][CH2:7][OH:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 24408BromineHCID 787243-Methoxyphenethyl alcohol

Produkt 1

HCID 104896782-(2-BROMO-5-METHOXYPHENYL)ETHANOLAusbeute 83,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a stirred mixture of 3-methoxyphenethyl alcohol (1.18 g, 7.8 mmol) and pyridine (0.75 ml, 9.3 mmol) in dry dichloromethane (10 ml) was added bromine (0.47 ml, 18.0 mmol) dropwise under nitrogen at 0° C. The orange solution was stirred at room temperature for 4 hours (hr). The reaction mixture was quenched by the addition of 10% sodium bisulfite aqueous solution., and extracted with dichloromethane. The organic extracts were washed with brine, dried over magnesium sulfate, and concentrated to give crude products, which were purified by silica-gel column chromatography eluted with gradient of hexane and ethyl acetate (10:1, 8:1, 5:1) to give the title compound as a colorless oil (1.5 g, 83.2%). 1H-NMR (CDCl3): 7.43 (d, J=8.8 Hz, 1H), 6.83 (d, J=3.3 Hz, 1H), 6.67 (dd, J=8,8, 3.3 Hz, 1H), 3.91-3.81 (m, 2H), 3.78 (s, 3H), 2.99 (t, J=6.6 Hz, 2H).

Aufarbeitung

  1. customThe reaction mixture was quenched by the addition of 10% sodium bisulfite aqueous solution
  2. extraction, and extracted with dichloromethane
  3. washThe organic extracts were washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customto give crude products, which
  7. customwere purified by silica-gel column chromatography
  8. washeluted with gradient of hexane and ethyl acetate (10:1, 8:1, 5:1)

Quellen und Nachweise

ORD-Eintrag
ord-7b04892886ad4946b33bf4feef0143fa
Quelldatensatz
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06239147B1

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