Potassium Hydroxide → 9-Methylene-9H-fluorene

HRID 2253256

Reaktionsgleichung

Reaktionsgleichung von HRID 2253256
O[CH2:2][CH:3]1[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2.[OH-].[K+]>CO>[CH2:2]=[C:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[C:10]2[C:15]1=[CH:14][CH:13]=[CH:12][CH:11]=2

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 904669H-Fluorene-9-methanol

Produkt 1

HCID 781479-Methylene-9H-fluorene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

9-Hydroxymethylfluorene (10 g) and 1 g KOH were dissolved in 90 ml of methanol and reacted at 60° C. for 1 hour, and the methanol was evaporated. From the solid thus obtained, dibenzofulvene was extracted using hexane and water, and washed with water until the hexane phase containing dibenzofulvene was neutral. After separating off the hexane phase, the hexane was evaporated, and the solid obtained was recrystallized from a mixed solvent of hexane-diethyl ether (4/6 v/v) to obtain dibenzofulvene. The melting point of the dibenzofulvene was 50-52° C.

Aufarbeitung

  1. customreacted at 60° C. for 1 hour
  2. customthe methanol was evaporated
  3. customFrom the solid thus obtained
  4. extractiondibenzofulvene was extracted
  5. washwashed with water until the hexane phase
  6. additioncontaining dibenzofulvene
  7. customAfter separating off the hexane phase
  8. customthe hexane was evaporated
  9. customthe solid obtained
  10. customwas recrystallized from a mixed solvent of hexane-diethyl ether (4/6 v/v)

Quellen und Nachweise

ORD-Eintrag
ord-ee04c424bba046deb80f0f60b96dd9f3
Quelldatensatz
uspto-grants-2008_01
Patentnummer
US07323538B2

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