Chloroform → HCID 68521334, Verbindung

HRID 2384520Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2384520
[Br:1][C:2]1[C:10]2[C:5](=[N+:6]([O-])[CH:7]=[C:8]([N+:11]([O-])=O)[CH:9]=2)[S:4][C:3]=1[S:15]([C:18]1[CH:23]=[C:22]([F:24])[CH:21]=[C:20]([C:25]#[N:26])[CH:19]=1)(=[O:17])=[O:16].C(Cl)(Cl)Cl>C(O)(=O)C.[Fe]>[NH2:11][C:8]1[CH:9]=[C:10]2[C:2]([Br:1])=[C:3]([S:15]([C:18]3[CH:23]=[C:22]([F:24])[CH:21]=[C:20]([C:25]#[N:26])[CH:19]=3)(=[O:16])=[O:17])[S:4][C:5]2=[N:6][CH:7]=1

Komponenten

5

Edukt 2

HCID 6212ChloroformHCID 68519824HCID 68519824, Verbindung

Produkt 1

HCID 68521334HCID 68521334, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

3-Bromo-2-(3-cyano-5-fluoro-benzenesulfonyl)-5-nitro-thieno[2,3-b]pyridin-N-oxide (1.0 g, 2.18 mmol) was suspended in acetic acid (12 ml) and Fe powder was added (0.73 g, 13 mmol). The reaction mixture was stirred at 60-70° C. for 60 minutes. Chloroform (45 ml) was added and after filtration through celite the filtrate was evaporated, the crude residue was treated with methanol (3 ml). The product was filtered, washed with methanol. It was obtained (0.69 g, 76.7%) as a yellow powder. LC-MS: (M+H)+ 413.1.

Aufarbeitung

  1. filtrationafter filtration through celite the filtrate
  2. customwas evaporated
  3. additionthe crude residue was treated with methanol (3 ml)
  4. filtrationThe product was filtered
  5. washwashed with methanol
  6. customIt was obtained (0.69 g, 76.7%) as a yellow powder

Quellen und Nachweise

ORD-Eintrag
ord-5447f3b459614853822be6549a6b67cc
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08263773B2

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