Acetic Acid → HCID 178476732, Verbindung

HRID 869450Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869450
[N:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[N+:6]([O-])[C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:12]([OH:15])(=[O:14])[CH3:13]>N1C=CC=CC=1.[Fe]>[C:12]([OH:15])(=[O:14])[CH3:13].[N:1]1[C:10]2[C:5](=[N:6][CH:7]=[CH:8][CH:9]=2)[C:4]([OH:14])=[CH:3][CH:2]=1

Komponenten

5

Edukt 2

HCID 176Acetic AcidHCID 3392321-Oxo-1lambda~5~-1,5-naphthyridine

Produkt 1

HCID 178476732HCID 178476732, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 1049PyridineLösungsmittel

Versuchsvorschrift

To a solution of 1,5-naphthyridin-5-oxide 4-01 (D-5) (330 mg, 2.0 mmol, 1.0 eq) in acetic acid (12 mL) and pyridine (2.5 mL) at RT, iron powder (456 mg, 8.15 mmol, 4.0 eq) is added in portions (over 10 min) and the resulting mixture is stirred for 2 h. The mixture is filtered and the solid is rinsed with acetic acid. The filtrate is concentrated in vacuo. The residue is triturated with acetone and then filtered. The filter cake is rinsed with acetone and dried in vacuo to afford the product, 1,5-naphthyridin-4-ol acetic acid salt (D-6).

Aufarbeitung

  1. filtrationThe mixture is filtered
  2. washthe solid is rinsed with acetic acid
  3. concentrationThe filtrate is concentrated in vacuo
  4. customThe residue is triturated with acetone
  5. filtrationfiltered
  6. washThe filter cake is rinsed with acetone
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d92b4189a0ae44c4877aabd49bd8f0f2
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969363B2

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