Reaktion #77418

Reaktionsgleichung

2-bromo-6-thioureidopyridine

chloroacetaldehyde

→

titled compound

Ausbeute 96.0%

6-Bromo-N-(2-thiazolyl)pyridin-2-amine

Ausbeute 96.0%

Lösungsmittel

ethanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturat reflux for 4.75 h
3. 3
   EinengenThe solution was concentrated in vacuo
4. 4
   workup.ADDITIONthe residue was diluted with 1 N aqueous NaOH solution at 0° C.
5. 5
   workup.ADDITIONthe pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution
6. 6
   FiltrationThe precipitate was collected by filtration
7. 7
   Waschenwashed several times with water
8. 8
   Trocknendried in vacuo over P2O5

Vorschrift

A suspension of 2-bromo-6-thioureidopyridine (3 g, 12.92 mmol) and chloroacetaldehyde (3.28 mL, 25.85 mmol) in ethanol (27 mL) and water (7 mL) was heated at reflux for 4.75 h. The solution was concentrated in vacuo and the residue was diluted with 1 N aqueous NaOH solution at 0° C., stirred for 10 min, and the pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution. The precipitate was collected by filtration, washed several times with water and dried in vacuo over P2O5 to obtain the titled compound (3.17 g, 96%) as a light yellow solid.

Quelle