Phosphorus tribromide → HCID 22494096, Verbindung

HRID 1816631Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1816631
O[CH2:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:21])[CH3:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].P(Br)(Br)[Br:23]>C(COC)OC.CCOCC>[Br:23][CH2:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:21])[CH3:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

5

Edukt 2

HCID 24614Phosphorus tribromideHCID 22494341HCID 22494341, Verbindung

Produkt 1

HCID 22494096HCID 22494096, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

2.2 g of ethyl 3-[3-(hydroxymethyl)-4-methoxyphenyl]-2-isopropoxypropanoate was dissolved in 15 ml dimethoxyethane. 1.2 ml phosphorus tribromide was added thereto under ice-cooling, followed by stirring at room temperature for 4 hours. The reaction solution was diluted with ether and washed with water. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and the solvent was evapoarated. The residue was subjected to silica gel column chromatography, to give 2.6 g of ethyl 3-[3-(bromomethyl)-4-methoxyphenyl]-2-isopropoxypropanoate from fractions eluted with hexane-ethyl acetate (4:1).

Aufarbeitung

  1. temperatureunder ice-cooling
  2. washwashed with water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-503ae909041e4040a24f0d42193a730b
Quelldatensatz
uspto-grants-2005_04
Patentnummer
US06884821B1

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