Methyl iodide → HCID 178493240, Verbindung

HRID 1803177Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1803177
[I:1][CH3:2].[F:3][C:4]1[CH:5]=[C:6]([NH:18][C:19]([NH2:21])=[S:20])[CH:7]=[C:8]([O:16][CH3:17])[C:9]=1[N:10]1[CH:14]=[N:13][C:12]([CH3:15])=[N:11]1>C(O)C>[IH:1].[F:3][C:4]1[CH:5]=[C:6]([NH:18][C:19]([S:20][CH3:2])=[NH:21])[CH:7]=[C:8]([O:16][CH3:17])[C:9]=1[N:10]1[CH:14]=[N:13][C:12]([CH3:15])=[N:11]1

Komponenten

4

Edukt 2

HCID 6328Methyl iodideHCID 866499201-(3-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea

Produkt 1

HCID 178493240HCID 178493240, VerbindungAusbeute 99,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Step S (4): Iodomethane (0.179 mL, 2.88 mmol) was added to a solution of 1-(3-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (0.772 g, 2.74 mmol) in absolute ethanol (50 mL). The resulting mixture was heated at 70° C. for 3 h. The crude reaction mixture was concentrated in vacuo. The residual solid was dried under high vacuum to afford methyl 3-fluoro-5-methoxy-4-(3-methyl-1H-1,2,4-triazol-1-yl)phenylcarbamimidothioate, hydroiodide (1.15 g, 2.72 mmol, 99% yield) as a yellow solid. LC-MS (M+H)+ 296.1.

Aufarbeitung

  1. customThe crude reaction mixture
  2. concentrationwas concentrated in vacuo
  3. customThe residual solid was dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-eb644a26475e419f8d247f06e7ba21db
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08349880B2

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