StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

1-[3-(3,4-Dichloro-benzyloxy)-phenyl]-ethanone → 2-Bromo-1-[3-(3,4-dichloro-benzyloxy)-phenyl]-ethanone

HRID 879719
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 879719
[Cl:1][C:2]1[CH:3]=[C:4]([CH:16]=[CH:17][C:18]=1[Cl:19])[CH2:5][O:6][C:7]1[CH:8]=[C:9]([C:13](=[O:15])[CH3:14])[CH:10]=[CH:11][CH:12]=1.C1CNC(=O)C1.[Br:26][Br-]Br>CO.C(Cl)Cl>[Br:26][CH2:14][C:13]([C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([O:6][CH2:5][C:4]2[CH:16]=[CH:17][C:18]([Cl:19])=[C:2]([Cl:1])[CH:3]=2)[CH:8]=1)=[O:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 288256531-[3-(3,4-Dichloro-benzyloxy)-phenyl]-ethanone

Produkt 1

HCID 583275612-Bromo-1-[3-(3,4-dichloro-benzyloxy)-phenyl]-ethanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21226129Dichloromethane methanolLösungsmittel

Versuchsvorschrift

1-[3-(3,4-Dichloro-benzyloxy)-phenyl]-ethanone (30 g) was dissolved in MeOH:DCM (2:1, 300 mL) and pyrolidone hydrotribromide (75 g) was added portion wise and stirred at room temperature for 3 hours. After completion of the reaction, the mixture was concentrated in vacuo and poured into saturated sodium bicarbonate solution (200 mL) and extracted with ethyl acetate (2×200 mL). The organic extracts were combined and washed with brine and concentrated in vacuo. Then this residue was dissolved in DCM (75 mL) and product was precipitated by slow addition of methanol (75 mL), filtered and dried in vacuum (29 g). 1H NMR (400 MHz, CDCl3): 7.62-7.54 (m, 3H), 7.47 (d, 1H), 7.42 (t, 1H), 7.25-7.30 (m, 1H), 7.18-7.23 (m, 1H), 5.07 (s, 2H), 4.44 (s, 2H).

Aufarbeitung

  1. customAfter completion of the reaction
  2. concentrationthe mixture was concentrated in vacuo
  3. additionpoured into saturated sodium bicarbonate solution (200 mL)
  4. extractionextracted with ethyl acetate (2×200 mL)
  5. washwashed with brine
  6. concentrationconcentrated in vacuo
  7. dissolutionThen this residue was dissolved in DCM (75 mL)
  8. customproduct was precipitated by slow addition of methanol (75 mL)
  9. filtrationfiltered
  10. customdried in vacuum (29 g)

Quellen und Nachweise

ORD-Eintrag
ord-91bfaea4f3914b589da54ae6946c14b6
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08987295B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion