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HCID 629261, Verbindung → HCID 14547484, Verbindung

HRID 979576
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 979576
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11](Br)=[C:10](Br)[S:9][C:8]=2[CH:14]=1)(=[O:3])[CH3:2]>C(O)C.C(OCC)(=O)C>[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[CH:11]=[CH:10][S:9][C:8]=2[CH:14]=1)(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 629261HCID 629261, Verbindung

Produkt 1

HCID 14547484HCID 14547484, VerbindungAusbeute 107,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

6-Acetyl-2,3-dibromobenzo[b]thiophene (6.68 g, 20 mmole) was dissolved in a mixture of ethanol and ethyl acetate (100 ml each) and MgO (1.6 g) and (20% Pd(OH2)/C (800 mg) were added under a N2 atmosphere. Hydrogenolysis was carried out at 40 psi of H2 at room temperature for 3 hours. The catalyst was removed by filtration and the solvent was removed in vacuo. The residue was partitioned between CHCl3 (100 ml) and H2O (50 ml). The CHCl3 layer was washed with H2O (50 ml). The aqueous layers were combined and back-extracted with CHCl3 (30 ml). The CHCl3 solutions were combined, dried over Na2SO4 and the solvent evaporated in vacuo to yield 3.8 g of product which was used in the next step without further purification.

Aufarbeitung

  1. customThe catalyst was removed by filtration
  2. customthe solvent was removed in vacuo
  3. customThe residue was partitioned between CHCl3 (100 ml) and H2O (50 ml)
  4. washThe CHCl3 layer was washed with H2O (50 ml)
  5. extractionback-extracted with CHCl3 (30 ml)
  6. dry with materialdried over Na2SO4
  7. customthe solvent evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-77f070222e4c441db19e7afe4a7ac116
Quelldatensatz
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04668697

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