2-Pyridinamine, 5-iodo- → HCID 77985000、化合物
反応式
Br[CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)=[N:9][CH:10]=1)=O.[NH2:16][C:17]1[CH:22]=[CH:21][C:20]([I:23])=[CH:19][N:18]=1>C(#N)C>[N:11]1([C:8]2[CH:7]=[CH:6][C:5]([C:3]3[N:16]=[C:17]4[CH:22]=[CH:21][C:20]([I:23])=[CH:19][N:18]4[CH:2]=3)=[CH:10][N:9]=2)[CH:15]=[CH:14][CH:13]=[N:12]1参加物
4
反応条件
- 温度
- 100 °C
実験手順
100.0 mg (corresponding to 0.38 mmol) of 5-(2-bromoacetyl)-2-(pyrazole-1-yl)pyridine and 83.6 mg (corresponding to 0.38 mmol) of 2-amino-5-iodopyridine were dissolved in 3.8 mL of acetonitrile. The resulting solution was heated under reflux for 4 hours in an oil bath at 100° C. After the completion of the reaction, the reaction solution was cooled down to room temperature, and precipitates were filtered. The precipitates were washed with acetonitrile and dried under reduced pressure. The resulting crude crystals were suspended in a mixed solution of 50 mL of water and 50 mL of methanol. Then, about 50 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for an hour using an ultrasonic washing machine. Precipitates were filtered from the resulting mixture, sufficiently washed with water, and dried under reduced pressure, to obtain 80.2 mg (corresponding to 0.21 mmol) of 2-[2-(pyrazole-1-yl)pyridine-5-yl]-6-iodoimidazo[1,2-a]pyridine (FIG. 5, step 3).