Stannous chloride dihydrate → 7-Chloro-3,4-dihydro-6-methyl-2(1H)-quinoxalinone

HRID 1600716Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1600716
[Na+].[Cl:2][C:3]1[C:8]([CH3:9])=[CH:7][C:6]([NH:10][CH2:11][C:12]([O-])=[O:13])=[C:5]([N+:15]([O-])=O)[CH:4]=1.O.O.[Sn](Cl)Cl>C(O)C>[Cl:2][C:3]1[CH:4]=[C:5]2[C:6]([NH:10][CH2:11][C:12](=[O:13])[NH:15]2)=[CH:7][C:8]=1[CH3:9]

Komponenten

4

Edukt 2

HCID 61436Stannous chloride dihydrateHCID 21189951HCID 21189951, Verbindung

Produkt 1

HCID 100814077-Chloro-3,4-dihydro-6-methyl-2(1H)-quinoxalinoneAusbeute 66,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of N-(4'chloro-5'-methyl-2'-nitrophenyl)glycine sodium salt (0.300 g, 1.23 mmol, as prepared above) and tin (II) chloride dihydrate (0.830 g, 3.68 mmol, Aldrich, used as received) in ethanol (4.0 mL) was refluxed for 30 min. It was then cooled to room temperature and the precipitated solid was filtered, washed with ethanol (1.0 mL) and dried under vacuum to yield 0.160 g (66%) of the title compound as a yellow powder; 1H NMR (DMSO-d6): δ 2.099 (s, 3H), 3.655 (s, 2H), 6.037 (s, 1H), 6.538 (s, 1H), 6.685 (s, 1H), 10.241 (s, 1H).

Aufarbeitung

  1. filtrationthe precipitated solid was filtered
  2. washwashed with ethanol (1.0 mL)
  3. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-e46b6d533d404ac584626cd73b4c9ab5
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05977107

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