StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrogen Peroxide → 9h-Fluoren-2-yl acetate

HRID 2416351
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2416351
S(=O)(=O)(O)O.C([C:9]1[CH:21]=[CH:20][C:19]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:12][C:11]=2[CH:10]=1)(=O)C.[C:22]([O:25]C(=O)C)(=[O:24])[CH3:23].OO>O.C(O)=O>[C:22]([O:25][C:9]1[CH:21]=[CH:20][C:19]2[C:14]3[C:13](=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:12][C:11]=2[CH:10]=1)(=[O:24])[CH3:23]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 699082-Acetylfluorene

Produkt 1

HCID 2470609h-Fluoren-2-yl acetateAusbeute 83,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 284Formic Acid
Lösungsmittel
HCID 962WaterLösungsmittel

Versuchsvorschrift

Sulfuric acid (40 mL) was added to a mixture of 2-acetylfluorene (165 g), formic acid (320 g), acetic anhydride (120 g) and dicholoromethane (1 L), and then aqueous hydrogen peroxide (120 mL) was dropwise added thereto. The solution was stirred for 30 minutes at a room temperature, and it was heated up to 40° C. and further stirred for 5 hours. Water (1 L) was added to the reaction mixture, and the dichloromethane layer was separated. The dichloromethane layer was washed in order with a saturated sodium carbonate aqueous solution, a sodium hydrogensulfite aqueous solution and water, and then it was dried on anhydrous magnesium sulfate and concentrated to obtain a solid matter. This was recrystallized from a mixed solvent of heptane-ethyl acetate (1:1) to obtain 2-acetoxyfluorene (149 g) of colorless needle crystal. The melting point was 130 C.

Aufarbeitung

  1. temperatureit was heated up to 40° C.
  2. stirringfurther stirred for 5 hours
  3. customthe dichloromethane layer was separated
  4. washThe dichloromethane layer was washed in order with a saturated sodium carbonate aqueous solution
  5. dry with materiala sodium hydrogensulfite aqueous solution and water, and then it was dried on anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto obtain a solid matter
  8. customThis was recrystallized from a mixed solvent of heptane-ethyl acetate (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-0ea5664139024967b164e558b7400518
Quelldatensatz
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06824709B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion