Methyl iodide → HCID 178512035, Verbindung

HRID 499799Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 499799
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=S)=[CH:4][CH:3]=1.CI.[N:17]#[C:18][NH2:19].O.NN>CC#N>[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10]/[C:9]/2=[N:19]\[C:18]#[N:17])=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 6328Methyl iodideHCID 9864CyanamideHCID 24654Hydrazine hydrate (1:1)HCID 86616333HCID 86616333, Verbindung

Produkt 1

HCID 178512035HCID 178512035, VerbindungAusbeute 13,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

To a solution of 1-(4-iodophenyl)pyridine-2(1H)-thione (180 mg, 0.575 mmol) in CH3CN (15 mL), CH3I (0.50 mL, 8.0 mmol) was added. After being stirred at room temperature overnight, the mixture was concentrated in vacuo to give a solid. The solid was dissolved in CH3CN (5 mL). To the solution, cyanamide (200 mg, 4.76 mmol) and hydrazine monohydrate (0.100 mL, 2.06 mmol) were added. After being stirred at room temperature for 2 h, the mixture was purified by HPLC to give (E)-(1-(4-iodophenyl)pyridin-2(1H)-ylidene)cyanamide (25 mg).

Aufarbeitung

  1. concentrationthe mixture was concentrated in vacuo
  2. customto give a solid
  3. stirringAfter being stirred at room temperature for 2 h
  4. customthe mixture was purified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-78e284f3339045caa9a014e899353d75
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07767697B2

Notizen zur Reaktion

Wird geladen…