反応 #1320

反応方程式

sodium iodide

hydriodic acid

6-chloronicotinic acid

→

title compound

6-Iodonicotinic acid

溶媒

acetone

反応条件

後処理

1. 1
   温度to warm slightly
2. 2
   workup.STIRRINGwith stirring
3. 3
   温度heated at 120°-125° C. in an oil bath for 42 hours
4. 4
   その他A dark brown layer formed above the yellow solid material
5. 5
   温度to cool to room temperature
6. 6
   ろ過The resultant yellow solid was collected by filtration
7. 7
   洗浄washed with 200 ml of 1N NaHSO3 solution
8. 8
   その他dried in high vacuum (3 mm Hg)

実験手順

To 27.97 g (186.6 mmol) of sodium iodide cooled to -78° C. was added 121.77 g (71.6 ml, 952.0 mmol) of hydriodic acid (57 wt %). The reaction mixture was allowed to warm slightly with stirring for 5 minutes, and then 30.00 g (190.4 mmol) of 6-chloronicotinic acid was added. The resulting mixture was allowed to warm to room temperature with stirring and then heated at 120°-125° C. in an oil bath for 42 hours. A dark brown layer formed above the yellow solid material. The reaction mixture was allowed to cool to room temperature and then poured into acetone (chilled to 0° C.). The resultant yellow solid was collected by filtration, washed with 200 ml of 1N NaHSO3 solution, and dried in high vacuum (3 mm Hg) to give the title compound as a pale yellow solid.

出典