Thionyl Chloride → HCID 10035354, Verbindung

HRID 1534419Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1534419
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:5][CH2:6]O.S(Cl)([Cl:15])=O>C(Cl)Cl>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:5][CH2:6][Cl:15]

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 100349915-(2-Hydroxyethyl)-2-methoxyphenol

Produkt 1

HCID 10035354HCID 10035354, VerbindungAusbeute 33 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 3-hydroxy-4-methoxyphenethyl alcohol (2.25 g) and thionyl chloride (5 ml) in methylene chloride (120 ml) was heated under reflux for 16 hours and evaporated. The residue was azeotroped twice with hexane and purified by chromatography on silica (30 g) using methylene chloride plus 0-6% methanol as the eluant. Appropriate fractions were combined and evaporated to give the title compound as a colourless solid (0.82 g, 33%), m.p. 53°-54°, which was characterised by its 1H-n.m.r. spectrum.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. customevaporated
  4. customThe residue was azeotroped twice with hexane
  5. custompurified by chromatography on silica (30 g)
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-56d2b0da3af145f2a526f46e6ee93563
Quelldatensatz
uspto-grants-1992_02
Patentnummer
US05089505

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