反应详情

温度

120 °C

To 5-bromo-3-amino-2-nitropyridine (190 mg, 0.872 mmol) in a dry microwave reaction tube were added phenylboronic acid (159 mg, 1.31), K2CO3 (361 mg, 2.61 mmol) and Pd(PPh3)4 (101 mg, 0.087 mmol) and the reaction flask was evacuated and flushed with N2 four times. To this solid reaction mixture was added anhydrous THF (2 mL) and the reaction mixture was degassed by applying vacuum and flushing with N2 five times and sealed in N2 atmosphere. The reaction mixture was then heated 120° C. for 2 h. After this time, LC/MS analysis of the reaction mixture should essentially show the desired product. Reaction mixture was concentrated in vacuo and to the residue was added MeOH and stirred for 30 min. All the solids were collected by filtration and washed thoroughly with MeOH and water MS: cal'd 216 (M+H)+, exp 216 (M+H)+

1. customthe reaction flask was evacuated
2. customflushed with N2 four times
3. customTo this solid reaction mixture
4. customthe reaction mixture was degassed
5. customflushing with N2 five times
6. customsealed in N2 atmosphere
7. customReaction mixture
8. concentrationwas concentrated in vacuo and to the residue
9. additionwas added MeOH
10. filtrationAll the solids were collected by filtration
11. washwashed thoroughly with MeOH and water MS