Potassium Carbonate → HCID 21453224, Verbindung

HRID 436601Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 436601
[CH2:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[OH:11])[CH:2]=[CH2:3].Cl[CH2:13][CH2:14][CH2:15][N:16]1[CH2:32][CH2:31][C:19]2([N:23]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:22][NH:21][C:20]2=[O:30])[CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH2:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[O:11][CH2:13][CH2:14][CH2:15][N:16]1[CH2:17][CH2:18][C:19]2([N:23]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:22][NH:21][C:20]2=[O:30])[CH2:31][CH2:32]1)[CH:2]=[CH2:3]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 113441122-Allyl-4-fluorophenolHCID 21453222HCID 21453222, Verbindung

Produkt 1

HCID 21453224HCID 21453224, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 1.5 g of 2-allyl-4-fluorophenol, 3.1 g of 8-(3-chloropropyl)-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, 0.7 g of potassium carbonate and 40 ml of toluene was heated under reflux for 10 hours. After cooling, the reaction mixture was washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with ether, cooled and filtered to give 8-{3-(2-allyl-4-fluorophenoxy)propyl}-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, m.p. 110° - 113° C; recrystallized from cyclohexane, m.p. 117° - 117.5° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 10 hours
  3. temperatureAfter cooling
  4. washthe reaction mixture was washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue was triturated with ether
  8. temperaturecooled
  9. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-890635a35dfe40ce913a0d17b80ad267
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04009275

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