反応 #77418

反応方程式

2-bromo-6-thioureidopyridine

chloroacetaldehyde

→

titled compound

収率 96.0%

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

収率 96.0%

溶媒

ethanol

water

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 4.75 h
3. 3
   濃縮The 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
   ろ過The precipitate was collected by filtration
7. 7
   洗浄washed several times with water
8. 8
   乾燥dried in vacuo over P2O5

実験手順

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.

出典