Sulfuric acid magnesium salt (1:1) → HCID 12507349, Verbindung

HRID 728533Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 728533
[Cl:1][C:2]1([Cl:11])[C@H:9]2[C@H:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C@@H:3]1[OH:10].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[Cl:1][C:2]1([Cl:11])[C@H:9]2[C@H:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C:3]1=[O:10]

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 14127271HCID 14127271, VerbindungHCID 178418287HCID 178418287, Verbindung

Produkt 1

HCID 12507349HCID 12507349, VerbindungAusbeute 80,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 3.9 g of (1R,6S,7S)-8,8-dichlorobicyclo [4.2.0]oct-2-en-7-ol, prepared as shown in Example 1, 9.0 g of pyridinium chlorochromate and 14 g of magnesium sulfate in 200 ml of methylene chloride under nitrogen was refluxed for 4 hours. The mixture was cooled, filtered first through celite then Florisil. Solvent was removed from the eluate under reduced pressure and the residue distilled under vacuum to give 3.1 g of (1R,6S)-8,8-dichlorobicyclo[4.2.0]oct-2-en-7-one, [α]D =+71.4°, (C=0.7, CHCl3).

Aufarbeitung

  1. customprepared
  2. temperaturewas refluxed for 4 hours
  3. temperatureThe mixture was cooled
  4. filtrationfiltered first through celite
  5. customSolvent was removed from the eluate under reduced pressure
  6. distillationthe residue distilled under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-c261590a3987480692eda02152f68240
Quelldatensatz
uspto-grants-1991_09
Patentnummer
US05049497

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