Potassium Hydroxide → HCID 21503899, Verbindung

HRID 1077305Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1077305
[C:1]([C:6]1[CH:18]=[CH:17][C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][C:8]=2[CH:7]=1)(=O)[CH2:2][CH2:3][CH3:4].[OH-].[K+].O.NN>C(O)CO>[CH2:1]([C:6]1[CH:18]=[CH:17][C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][C:8]=2[CH:7]=1)[CH2:2][CH2:3][CH3:4]

Komponenten

5

Edukt 3

HCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 125571201-(9H-Fluoren-2-yl)butan-1-one

Produkt 1

HCID 21503899HCID 21503899, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 174Ethylene GlycolLösungsmittel

Versuchsvorschrift

A mixture of 2-butyrylfluorene (11.3 g.), powdered potassium hydroxide (4.16 g.) and 100% hydrazine hydrate (9 ml.) in ethylene glycol (104 ml.) was refluxed for one hour with stirring. The mixture was then slowly distilled until the boiling-point reached 185° and then heated to reflux for 3 hours. The cooled mixture was treated with water (ca. 300 ml.) and the produce was isolated with ether in the usual manner. Recrystallisation from methanol gave 2-butyfluorene, m.p. 65°-66.5° .

Aufarbeitung

  1. temperaturewas refluxed for one hour
  2. distillationThe mixture was then slowly distilled until the boiling-point
  3. customreached 185°
  4. temperatureheated
  5. temperatureto reflux for 3 hours
  6. additionThe cooled mixture was treated with water (ca. 300 ml.)
  7. customthe produce was isolated with ether in the usual manner
  8. customRecrystallisation from methanol

Quellen und Nachweise

ORD-Eintrag
ord-2db241d206c14384b0654db26de4ba5c
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03959482

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