N-Iodosuccinimide → HCID 23449208, Verbindung

HRID 1839331Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1839331
[I:1]N1C(=O)CCC1=O.[CH3:9][S:10][C:11]1[N:12]=[CH:13][N:14]2[CH:18]=[CH:17][S:16][C:15]=12>ClCCl.[Cl-].[Na+].O>[I:1][C:13]1[N:14]2[C:15]([S:16][CH:17]=[CH:18]2)=[C:11]([S:10][CH3:9])[N:12]=1

Komponenten

5

Edukt 2

HCID 120273N-IodosuccinimideHCID 226315297-Methylthioimidazo[5,1-b]thiazole

Produkt 1

HCID 23449208HCID 23449208, VerbindungAusbeute 95,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

N-Iodosuccinimide (3.08 g) was added under ice cooling to a solution of 2.28 g of 7-methylthioimidazo[5,1-b]thiazole in dichloromethane. The mixture was stirred at room temperature for 7 hr. Saturated brine was added to the reaction mixture, followed by separation. The organic layer was washed with a dilute aqueous sodium thiosulfate solution and saturated brine in that order, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation. The residue was purified by column chromatography on silica gel (ethyl acetate:dichloromethane=1:1) to give 3.78 g of 5-iodo-7-methylthioimidazo[5,1-b]thiazole.

Aufarbeitung

  1. customfollowed by separation
  2. washThe organic layer was washed with a dilute aqueous sodium thiosulfate solution and saturated brine in that order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation
  5. customThe residue was purified by column chromatography on silica gel (ethyl acetate:dichloromethane=1:1)

Quellen und Nachweise

ORD-Eintrag
ord-1ac3c463b3684cecb09c58d033233cac
Quelldatensatz
uspto-grants-2004_01
Patentnummer
US06677331B2

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