反应详情

A mixture of 50 g. (0.44 mole) of 2-chloropyridine and 98.22 g. (0.88 mole) of semicarbazide hydrochloride in 150 ml. of 2-ethoxyethanol was heated to reflux and then treated with a solution of 1 ml. of concentrated sulfuric acid (36 N) in 5 ml. of 2-ethoxyethanol. The resulting solution was refluxed for 18 hr., cooled to about 60°, and treated with 150 ml. of water. The mixture was stirred, cooled to 0°, and kept 0.5 hr. and the solid was collected on a filter. The solid was washed well with water and dried under reduced pressure, to give 35.0 g (59%) of product, m.p. 230°-231°, which was sufficiently pure to be used for the next step.

1. additionA mixture of 50 g
2. temperatureto reflux
3. additiontreated with a solution of 1 ml
4. temperatureThe resulting solution was refluxed for 18 hr
5. temperature, cooled to about 60°
6. additiontreated with 150 ml
7. temperaturecooled to 0°
8. customand the solid was collected on a filter
9. washThe solid was washed well with water
10. customdried under reduced pressure