HCID 14769542, Verbindung → HCID 13577105, Verbindung

HRID 2286985Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2286985
[CH:1]([NH:3][C:4]1[S:8][N:7]=[C:6]([C:9](=[O:16])[CH:10](SC)[S:11]([CH3:13])=O)[N:5]=1)=[O:2].I([O-])(=O)(=O)=[O:18].[Na+]>C(O)(=O)C>[CH:1]([NH:3][C:4]1[S:8][N:7]=[C:6]([C:9](=[O:16])[C:10]([S:11][CH3:13])=[O:18])[N:5]=1)=[O:2]

Komponenten

4

Edukt 2

HCID 14769542HCID 14769542, VerbindungHCID 23667635Sodium periodate

Produkt 1

HCID 13577105HCID 13577105, VerbindungAusbeute 129,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 5-formamido-3-(2-methylthio-2-methylsulfinylacetyl)-1,2,4-thiadiazole (0.85 g) and sodium periodate (0.2 g) in glacial acetic acid (10 ml) was stirred for 45 minutes at 70° C. The reaction mixture was evaporated and the residue was dissolved in a mixture of ethyl acetate and water. The mixture was adjusted to pH 7 with an aqueous solution of sodium bicarbonate and treated with an aqueous solution of sodium thiosulfate. The organic layer was separated, dried over anhydrous magnesium sulfate and evaporated to dryness. The residue was triturated with a mixture of diethyl ether and petroleum ether to give the title compound (280 mg), mp. 186° to 187° C.

Aufarbeitung

  1. customThe reaction mixture was evaporated
  2. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
  3. additiontreated with an aqueous solution of sodium thiosulfate
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated to dryness
  7. customThe residue was triturated with a mixture of diethyl ether and petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-aba3668200d548f585189b113c163534
Quelldatensatz
uspto-grants-1981_05
Patentnummer
US04268509

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