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Xanthene → 2,7-Bis(4-chlorobutyryl)xanthene

HRID 1076901
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1076901
[CH:1]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[Cl:15][CH2:16][CH2:17][CH2:18][C:19](Cl)=[O:20].[Cl-:22].[Al+3].[Cl-].[Cl-]>C(Cl)Cl>[Cl:15][CH2:16][CH2:17][CH2:18][C:19]([C:10]1[CH:9]=[CH:8][C:7]2[O:6][C:5]3[C:14](=[CH:1][C:2]([C:5](=[O:6])[CH2:4][CH2:3][CH2:2][Cl:22])=[CH:3][CH:4]=3)[CH2:13][C:12]=2[CH:11]=1)=[O:20]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7107XantheneHCID 783704-Chlorobutyryl chlorideHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 123402802,7-Bis(4-chlorobutyryl)xanthene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

To a mixture of 91.1 g (0.5 mole) xanthene, 176.3 g (1.25 moles) of 4-chlorobutyryl chloride and 3 liters of dried methylene chloride cooled to -20°C. was added slowly over 1/2 hour 146.7 g (1.1moles) of aluminum chloride, maintaining a temperature below -10°C. The reaction mixture was allowed to warm slowly to room temperature and then refluxed for 4 hours and cooled to room temperature. The mixture was decomposed by pouring cautiously into 2 liters of ice water, and the layers were separated. The aqueous layer was extracted again with methylene chloride. The methylene chloride layers were combined and evaporated to a small volume and cooled. The resulting solid was filtered off and recrystallized from acetone to give the desired product. M.P. 131°-132°C.

Aufarbeitung

  1. temperaturemaintaining a temperature below -10°C
  2. temperatureto warm slowly to room temperature
  3. temperaturerefluxed for 4 hours
  4. temperaturecooled to room temperature
  5. customthe layers were separated
  6. extractionThe aqueous layer was extracted again with methylene chloride
  7. customevaporated to a small volume
  8. temperaturecooled
  9. filtrationThe resulting solid was filtered off
  10. customrecrystallized from acetone

Quellen und Nachweise

ORD-Eintrag
ord-68da17306fbd403a83123b0ac5c1f7da
Quelldatensatz
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03957989

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