Carbon tetrabromide → HCID 21476913, Verbindung

HRID 2293583Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2293583
O[CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]=1[CH2:13][CH2:14][CH3:15].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:36]>C(Cl)Cl>[Br:36][CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]=1[CH2:13][CH2:14][CH3:15]

Komponenten

5

Edukt 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 21476897HCID 21476897, Verbindung

Produkt 1

HCID 21476913HCID 21476913, VerbindungAusbeute 94,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a magnetically stirred solution of 0.405 g (1.94 mmol) of the product of Step D dissolved in 5.0 mL of methylene chloride was added 0.638 g (2.43 mmol) of triphenylphosphine followed by 0.806 g (2.43 mmol) of carbon tetrabromide at room temperature. The reaction mixture was stirred for 30 minutes at room temperature, then the magnetic stir bar was removed and the methylene chloride was evaporated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with 10% EtOAc-hexane, and evaporation of the purified fractions and solvent removal in vacuo afforded 0.496 g (94%) of the title compound.

Aufarbeitung

  1. customthe magnetic stir bar was removed
  2. customthe methylene chloride was evaporated in vacuo
  3. customThe residue was purified on a silica gel flash chromatography column
  4. washeluted with 10% EtOAc-hexane, and evaporation of the purified fractions and solvent removal in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1c48d9c1d6c946cda3fe851aca13b0e9
Quelldatensatz
uspto-grants-1997_11
Patentnummer
US05686478

Notizen zur Reaktion

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