m-Chloroperbenzoic acid → HCID 86755926, Verbindung

HRID 366284Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 366284
[CH3:1][O:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7][CH3:8].ClC1C=CC=C(C(OO)=[O:17])C=1>ClCCl>[CH2:7]([C@H:6]1[C@@H:5]([CH2:4][CH2:3][O:2][CH3:1])[O:17]1)[CH3:8]

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 5364230(3Z)-1-Methoxy-3-hexene

Produkt 1

HCID 86755926HCID 86755926, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

27.4 g of (Z)-1-methoxy-3-hexene were dissolved in dichloromethane (850 ml) and cooled to 10°. 62 g of ca 70% m-chloroperbenzoic acid corresponding to 1.05 eq., were added in portions. The mixture was allowed to react during 15 hours and was then transferred into an extraction funnel wherein it was washed with an aqueous solution of NaOH and then with water to neutrality. After separation and drying of the organic layer on Na2SO4, the residue was distilled over a 5 cm long Vigreux type column at 51-52°/1.5×103Pa to give 24.9 g (80%) of the desired compound in the form of a colourless liquid which presented the following analytical data:

Aufarbeitung

  1. temperaturecooled to 10°
  2. customto react during 15 hours
  3. customwas then transferred into an extraction funnel
  4. washwherein it was washed with an aqueous solution of NaOH
  5. customAfter separation
  6. customdrying of the organic layer on Na2SO4
  7. distillationthe residue was distilled over a 5 cm long Vigreux type column at 51-52°/1.5×103Pa

Quellen und Nachweise

ORD-Eintrag
ord-338e58e77cd24c89b0a9bce6c69402b7
Quelldatensatz
uspto-grants-2000_10
Patentnummer
US06129941

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