Methyl iodide → HCID 178504149, Verbindung

HRID 1594980

Reaktionsgleichung

Reaktionsgleichung von HRID 1594980
[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 ml). 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-7d8af54153e149f8b0ece54b8604e925
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06284777B1

Verknüpfte Notizen

Wird geladen…