Ethanol → 4-(4-Aminophenoxy)-2-butyrylaminopyridine

HRID 853457Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 853457
[C:1]([NH:6][C:7]1[CH:12]=[C:11]([O:13][C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][CH:15]=2)[CH:10]=[CH:9][N:8]=1)(=[O:5])[CH2:2][CH2:3][CH3:4].[Cl-].[NH4+].C(O)C.CN(C)C=O>[Fe].O>[NH2:20][C:17]1[CH:16]=[CH:15][C:14]([O:13][C:11]2[CH:10]=[CH:9][N:8]=[C:7]([NH:6][C:1](=[O:5])[CH2:2][CH2:3][CH3:4])[CH:12]=2)=[CH:19][CH:18]=1

Komponenten

7

Edukt 4

HCID 702EthanolHCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 229366772-Butyroylamino-4-(4-nitrophenoxy)pyridine

Produkt 1

HCID 229364634-(4-Aminophenoxy)-2-butyrylaminopyridine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 0.6 g of 2-butyrylamino-4-(4-nitrophenoxy)pyridine, 1.2 g of iron powder, 2.8 g of ammonium chloride, 10 ml of ethanol, 10 ml of dimethylformamide and 5 ml of water was vigorously stirred at 100° C. for 10 minutes. The reaction was filtered with celite, the solvent was distilled off under reduced pressure, and then water was added to the filtrate and extraction was performed with ethyl acetate. The extract was dried over magnesium sulfate and the solvent distilled off under reduced pressure to obtain 0.6 g of the target substance as a light yellow solid.

Aufarbeitung

  1. filtrationThe reaction was filtered with celite
  2. distillationthe solvent was distilled off under reduced pressure
  3. additionwater was added to the filtrate and extraction
  4. dry with materialThe extract was dried over magnesium sulfate
  5. distillationthe solvent distilled off under reduced pressure
  6. customto obtain 0.6 g of the target substance as a light yellow solid

Quellen und Nachweise

ORD-Eintrag
ord-81c4b0451e684897b689d131f1f3eb35
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07253286B2

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