反应 #2320124

反应方程式

6-bromo-3-methylpyridine

phenylboronic acid

triphenylphosphine

K2CO3

→

3-methyl-6-phenylpyridine

收率 84.1%

溶剂

dimethoxyethane

反应条件

后处理

1. 1
   温度The mixture was heated
2. 2
   温度at reflux for 20 hours
3. 3
   萃取The aqueous phase was extracted twice with 200 mL of ethyl acetate
4. 4
   萃取The combined organic extractions
5. 5
   萃取were then extracted with brine
6. 6
   干燥dried over magnesium sulfate
7. 7
   其他The filtrate was evaporated in vacuo
8. 8
   workup.DISTILLATIONthe resultant oil purified by Kugelehor distillation (190° C. @ 500 microns)

实验过程

To a 2 L flask, 45.0 g (262 mmol) of 6-bromo-3-methylpyridine, 38.3 g (314 mmol) of phenylboronic acid, 1.47 g (6.54 mmol) of palladium acetate, 6.86 g (26.2 mmol) of triphenylphosphine and 353 mL of 2M K2CO3 were added to 405 mL of dimethoxyethane. The mixture was heated at reflux for 20 hours and cooled to room temperature. The aqueous phase was extracted twice with 200 mL of ethyl acetate. The combined organic extractions were then extracted with brine and dried over magnesium sulfate. The filtrate was evaporated in vacuo and the resultant oil purified by Kugelehor distillation (190° C. @ 500 microns) to give 37.2 g (84.1% yield) of 3-methyl-6-phenylpyridine as white solids.

来源