Reacción #77417

Ecuación de reacción

potassium bicarbonate

2-bromo-6-benzoylthioureidopyridine

sodium hydroxide

HCl

→

titled compound

Rendimiento 94.0%

N-(6-Bromopyridin-2-yl)thiourea

Rendimiento 94.0%

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaunder reflux for an additional 10 min
2. 2
   TemperaturaThe mixture was cooled to 0° C.
3. 3
   workup.STIRRINGThe mixture was stirred at 0° C. for several min
4. 4
   Filtraciónthe precipitate was filtered
5. 5
   Lavadowashed several times with water
6. 6
   Secadodried in vacuo over P2O5

Procedimiento

A suspension of 2-bromo-6-benzoylthioureidopyridine (4.99 g, 14.84 mmol) in 10% aqueous sodium hydroxide solution (10.4 mL, 26 mmol) was stirred at rt. for 10 min and then under reflux for an additional 10 min. The mixture was cooled to 0° C. and acidified with 1 N aqueous HCl solution to pH 4.0 and then adjusted to pH 8.5 with satd. aqueous potassium bicarbonate solution. The mixture was stirred at 0° C. for several min and the precipitate was filtered, washed several times with water and dried in vacuo over P2O5 to obtain the titled compound (3.23 g, 94%) as a white solid.

Fuente