反応 #77417

反応方程式

potassium bicarbonate

2-bromo-6-benzoylthioureidopyridine

sodium hydroxide

HCl

→

titled compound

収率 94.0%

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

収率 94.0%

反応条件

後処理

1. 1
   温度under reflux for an additional 10 min
2. 2
   温度The mixture was cooled to 0° C.
3. 3
   workup.STIRRINGThe mixture was stirred at 0° C. for several min
4. 4
   ろ過the precipitate was filtered
5. 5
   洗浄washed several times with water
6. 6
   乾燥dried in vacuo over P2O5

実験手順

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.

出典