反应 #2146686
ord-4bc09b23fe4a40ff938a0b354a991ac2
反应方程式
反应条件
后处理
- 1其他After the completion of the reaction
- 2温度the reaction solution was cooled down to room temperature
- 3其他precipitates
- 4过滤were filtered
- 5其他recovered
- 6洗涤The precipitates were washed with acetonitrile
- 7其他dried under reduced pressure
- 8workup.ADDITIONThen, about 20 mL of a saturated sodium hydrogencarbonate solution was added
- 9其他the mixture was sonicated for 5 minutes
- 10其他Precipitates
- 11过滤were filtered
- 12其他recovered from the resulting mixture
- 13洗涤sufficiently washed with water
- 14其他dried under reduced pressure
实验过程
2.15 g (corresponding to 10.0 mmol) of 2-bromo-4′-hydroxyacetophenone and 1.25 g (corresponding to 10.0 mmol) of 2-amino-5-methoxypyridine were dissolved in 50 mL, of acetonitrile. The resulting solution was refluxed in an oil bath at 90° C. for 3.5 hours. After the completion of the reaction, the reaction solution was cooled down to room temperature, and precipitates were filtered and recovered. The precipitates were washed with acetonitrile and dried under reduced pressure. The resulting crude crystals were suspended in a mixed solution of 40 mL of water and 40 mL of methanol. Then, about 20 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for 5 minutes using a ultrasonic washing machine. Precipitates were filtered and recovered from the resulting mixture, sufficiently washed with water, and dried under reduced pressure, to obtain 1.96 g (corresponding to 8.16 mmol) of 2-(4′-hydroxyphenyl)-6-methoxyimidazo[1,2-a]pyridine (FIG. 2, Step 5).