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Sodium Carbonate → 1-[3-(p-Fluorobenzoyl)-propyl]-4,4-diphenylpiperidine

HRID 328250
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 328250
[C:1]1([C:7]2([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F:19][C:20]1[CH:31]=[CH:30][C:23]([C:24]([CH2:26][CH2:27][CH2:28]I)=[O:25])=[CH:22][CH:21]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(C(C)=O)C>[F:19][C:20]1[CH:21]=[CH:22][C:23]([C:24]([CH2:26][CH2:27][CH2:28][N:10]2[CH2:9][CH2:8][C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:12][CH2:11]2)=[O:25])=[CH:30][CH:31]=1
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Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 28232394,4-DiphenylpiperidineHCID 30162324'-Fluoro-4-iodobutyrophenone

Produkt 1

HCID 214360921-[3-(p-Fluorobenzoyl)-propyl]-4,4-diphenylpiperidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

6.1 g. of 4,4-diphenylpiperidine are heated to boiling with 6.2 g. of 3-(p-fluorobenzoyl)propyl iodide and 5.3 g of anhydrous sodium carbonate in 30 cc. of methyl ethyl ketone for 8 hours while stirring. After cooling, the precipitated salt is filtered off and the filtrate is evaporated to dryness. The residue is dissolved in water and the aqueous solution is rendered alkaline by the addition of sodium hydroxide solution. The resulting base is recovered by repeated extraction with ether. The combined ether extracts are dried over potassium carbonate, the ether is distilled off, and the residue is recrystallized from ethanol with the addition of activated charcoal. Thereby, 9 g. of 1-[3-(p-fluorobenzoyl)propyl] -4,4-diphenylpiperidine of the melting point 107° to 108° C. are obtained. On adding fumaric acid to its solution in ether, the furmarate of the melting point 195° to 197° C. is obtained.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe precipitated salt is filtered off
  3. customthe filtrate is evaporated to dryness
  4. dissolutionThe residue is dissolved in water
  5. additionby the addition of sodium hydroxide solution
  6. customThe resulting base is recovered
  7. extractionextraction with ether
  8. dry with materialThe combined ether extracts are dried over potassium carbonate
  9. distillationthe ether is distilled off
  10. customthe residue is recrystallized from ethanol with the addition of activated charcoal

Quellen und Nachweise

ORD-Eintrag
ord-802a1e58393c4759b50086142fcb2ab3
Quelldatensatz
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04016280

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