Ammonium Chloride → 1013117-35-5

HRID 2405758Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2405758
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-])=O)[N:8]=[CH:7][NH:6][C:5]2=[O:15].[NH4+].[Cl-]>CO.O.[Fe]>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[NH2:12])[N:8]=[CH:7][NH:6][C:5]2=[O:15]

Komponenten

6

Edukt 2

HCID 25517Ammonium ChlorideHCID 135767899HCID 135767899, Verbindung

Produkt 1

HCID 1360138721013117-35-5Ausbeute 100,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23925IronKatalysatorHCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

To a suspension of 6-chloro-7-nitroquinazoline-4-one (7.5 g, 33 mmol) in MeOH (250 mL) was added NH4Cl (17.7 g, 0.33 mol) dissolved in water (75 mL). Iron powder (18.5 g, 330 mmol) was added and the suspension was heated at 65° C. for 2 h. The warm reaction mixture was filtered over diatomaceous earth and washed several times with THF (1 L) and methanol (500 mL). The filtrate was concentrated, washed with water and dried under vacuum at 50° C. to afford the title compound (6.5 g, 90%) as a brown solid. ESI-MS m/z 196 [C8H6ClN3O+H]+.

Aufarbeitung

  1. customThe warm reaction mixture
  2. filtrationwas filtered over diatomaceous earth
  3. washwashed several times with THF (1 L) and methanol (500 mL)
  4. concentrationThe filtrate was concentrated
  5. washwashed with water
  6. customdried under vacuum at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-a111bca80fd34374af0fd0545523b698
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08809326B2

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