反应详情

A mixture of 2,3-dichloroisonicotinic acid ethyl ester (3.15 mmol), K2CO3 (4.73 mmol) and trimethylboroxine (3.15 mmol) in 4 mL dioxane was degassed with Ar. Then, tetrakis(triphenylphosphine)palladium (0.31 mmol) was added and the mixture was heated to reflux overnight. At RT, the reaction mixture was poured into water and extracted with DCM. The combined organic layers were dried over K2CO3, filtered over a pad of celite and concentrated in vacuo. Purification by CC (KP-SIL™ from Biotage) using Hept/EtOAc (8/2) gives the desired product as brown oil;

1. customwas degassed with Ar
2. temperaturethe mixture was heated
3. temperatureto reflux overnight
4. extractionextracted with DCM
5. dry with materialThe combined organic layers were dried over K2CO3
6. filtrationfiltered over a pad of celite
7. concentrationconcentrated in vacuo
8. customPurification by CC (KP-SIL™ from Biotage)