Tin atom → 7-Phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one

HRID 1509273Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1509273
[N+:1]([C:4]1[C:5]([O:16][CH2:17][C:18]([O:20]CC)=O)=[N:6][CH:7]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:9]=1)([O-])=O.[Sn]>Cl>[C:10]1([C:8]2[CH:7]=[N:6][C:5]3[O:16][CH2:17][C:18](=[O:20])[NH:1][C:4]=3[CH:9]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Komponenten

4

Edukt 2

HCID 5352426Tin atomHCID 67255179Ethyl 2-((3-nitro-5-phenylpyridin-2-yl)oxy)acetate

Produkt 1

HCID 669367437-Phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
2.5 °C

Versuchsvorschrift

In a 500 ml round-bottomed flask was added ethyl 2-(3-nitro-5-phenylpyridin-2-yloxy)acetate (4.6 g, 15.22 mmol) in hydrochloric acid, 37% (40 ml) to give a yellow suspension. The mixture was cooled to 0-5° C. followed by the portion wise addition of tin powder (9.94 g, 84 mmol). The addition proved to be exothermic. Caution should be taken while adding. The mixture was then stirred at room temperature for further 30 minutes until all foaming ceased. The reaction mixture was heated to 80° C. under a nitrogen atmosphere for 3 hours.

Aufarbeitung

  1. customto give a yellow suspension
  2. additionThe addition
  3. additionwhile adding
  4. temperatureThe reaction mixture was heated to 80° C. under a nitrogen atmosphere for 3 hours

Quellen und Nachweise

ORD-Eintrag
ord-f13cf9e9ce16442abb54db50a4d6fd1e
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09221838B2

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