Methyl iodide → HCID 178504149, Verbindung

HRID 412109

Reaktionsgleichung

Reaktionsgleichung von HRID 412109
[NH2:1][C:2]([NH:4][C:5]([NH2:7])=[S:6])=[S:3].[I:8][CH3:9]>C1COCC1.C1(C)C=CC=CC=1>[IH:8].[CH3:9][SH:3]=[C:2]([NH:4][C:5]([NH2:7])=[S:6])[NH2:1]

Komponenten

5

Edukt 2

HCID 6328Methyl iodideHCID 2758725Dithiobiuret

Produkt 1

HCID 178504149HCID 178504149, VerbindungAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirring solution of dithiobiuret (5.0 g, 37 mmol) in THF (75 mL) was added iodomethane (13.1 g, 92.5 mmol, 5.76 μl). After stirring at room temperature for 22 h, the solution was diluted with 150 mL of toluene and allowed to stand at 0° C. for 3 h. The crystals were collected by filtration and washed with cold 2:1 toluene/THF, then dried in vacuo to give the title compound as a white solid (8.7 g, 85%). MS(ESI): 149.9 (M+H)+.

Aufarbeitung

  1. waitto stand at 0° C. for 3 h
  2. filtrationThe crystals were collected by filtration
  3. washwashed with cold 2:1 toluene/THF
  4. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-51dd0600dffd46f4aa13bc0d38d80f27
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06562842B2

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