반응 #77418

반응 방정식

2-bromo-6-thioureidopyridine

chloroacetaldehyde

→

titled compound

수율 96.0%

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

수율 96.0%

용매

ethanol

water

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 4.75 h
3. 3
   농축The 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
   여과The precipitate was collected by filtration
7. 7
   세척washed several times with water
8. 8
   건조dried in vacuo over P2O5

실험 절차

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.

출처