Potassium Carbonate → HCID 57145772, Verbindung

HRID 1285134

Reaktionsgleichung

Reaktionsgleichung von HRID 1285134
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4](Cl)[N:3]=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([CH2:24][CH2:25][CH2:26][N:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)[O:23][CH2:22][CH2:21][O:20]2)=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)CC>[CH2:21]1[O:20][C:19]([C:16]2[CH:17]=[CH:18][C:13]([F:12])=[CH:14][CH:15]=2)([CH2:24][CH2:25][CH2:26][N:27]2[CH2:28][CH2:29][N:30]([C:4]3[N:3]=[C:2]([NH2:1])[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=3)[CH2:31][CH2:32]2)[O:23][CH2:22]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 27240356-Chloro-3-nitropyridin-2-ylamineHCID 27831211-(3-(2-(4-Fluorophenyl)-1,3-dioxolan-2-yl)propyl)piperazine

Produkt 1

HCID 57145772HCID 57145772, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10311-PropanolLösungsmittel

Versuchsvorschrift

5.6 g 2-amino-6-chloro-3-nitropyridine, 10 g 1-(3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl)piperazine, 5 g potassium carbonate and 100 ml n-propanol are refluxed 21/2 hours. After cooling the precipitate is filtered off. The filtrate is concentrated to ca. 10 ml and diluted with the same volume of diisopropyl ether. The resulting cristallisate is admixed with the above mentioned precipitate and partitioned between water and methylene chloride. The organic phase is filtered and evaporated to give the heading compound, m.p. 117°-118°.

Aufarbeitung

  1. temperatureAfter cooling the precipitate
  2. filtrationis filtered off
  3. concentrationThe filtrate is concentrated to ca. 10 ml
  4. additiondiluted with the same volume of diisopropyl ether
  5. custompartitioned between water and methylene chloride
  6. filtrationThe organic phase is filtered
  7. customevaporated
  8. customto give the heading compound, m.p. 117°-118°

Quellen und Nachweise

ORD-Eintrag
ord-c37eaf3eae08407a8b0553640c833c89
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04565816

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