Hydrochloric Acid → HCID 178474231, Verbindung

HRID 1112322Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1112322
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7](Br)[N+:6]=1[O-:12])(=[O:3])[CH3:2].[SH-:13].[Na+].Cl>C(O)C>[C:1]([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([SH:13])[N+:6]=1[O-:12])(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 28015Sodium hydrosulfideHCID 178474109HCID 178474109, Verbindung

Produkt 1

HCID 178474231HCID 178474231, VerbindungAusbeute 79 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

2 gms (0.0087 mole) of 2-acetamido-6-bromopyridine-1-oxide was suspended in 35 ml (0.035 mole) of 1M aqueous sodium hydrosulfide and 30 ml of ethanol and agitated at 60° C. for 5 hours and at room temperature one night. Concentrated hydrochloric acid was added dropwise to the cold yellow solution and the precipitated solid filtered, giving a 79% yield of 2-acetamido-6-mercaptopyridine-1-oxide. This impure product was purified by recrystallization from 2-propanol and hot filtration to remove a small amount of contaminating sulfur to give pale yellow crystals, m.p.=172.8°-173.5° C.

Aufarbeitung

  1. filtrationthe precipitated solid filtered

Quellen und Nachweise

ORD-Eintrag
ord-0fcaf14ee736481ea2e52c1b33a357dc
Quelldatensatz
uspto-grants-1978_10
Patentnummer
US04122085

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