Methyl iodide → HCID 178482153, Verbindung

HRID 559561Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 559561
[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.[CH3:17][NH2:18]>CC#N.CO>[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:18]\[CH3:17])=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 6328Methyl iodideHCID 6329MethylamineHCID 86616333HCID 86616333, Verbindung

Produkt 1

HCID 178482153HCID 178482153, VerbindungAusbeute 61,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 1-(4-iodophenyl)pyridine-2(1H)-thione (98 mg, 0.31 mmol) in CH3CN (5 mL), CH3I (0.25 mL, 4.0 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 MeOH (7 mL). To the solution, CH3NH2 (2M in THF, 0.80 mL, 1.6 mmol) was added. After being stirred at room temperature overnight, the mixture was purified by HPLC to give (E)-N-(1-(4-iodophenyl)pyridin-2(1H)-ylidene)methanamine (59 mg).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-f8405351e6004dc0b7d82dfca637ec8b
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08063077B2

Notizen zur Reaktion

Wird geladen…