反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 200 °C
PROCEDURE
实验过程
N-(3-(2,5-dichloropyrimidin-4-yl)phenyl)acrylamide (30 mg, 0.102 mmol), 4-(4-methylpiperazin-1-yl)aniline (21 mg, 0.110 mmol)) and potassium carbonate (14 mg, 0.101 mmol) were dissolved in toluene (4 mL) in a sealable microwave compatible reaction tube, then Pd2(dba)3 (2 mg, 0.002 mmol) and Xantphos (2.7 mg, 0.005 mmol) were added. The reaction tube was sealed and the reaction was heated under microwave irradiation (40 min, 200° C., 3 atm). The reaction was monitored by TLC. The product was purified by column chromatography (5% CH3OH/CH2Cl2) to give the title compound. 1H NMR (400 MHz, CD3OD): δ 8.40 (s, 1H), 8.20 (s, 1H), 7.77 (d, 1H, J=7.2 Hz), 7.59 (m, 3H), 7.46 (t, 1H, J=7.6 Hz), 6.96 (m, 2H), 6.46-6.36 (m, 2H), 5.79 (dd, 1H, J=2.4 & 9.6 Hz), 3.14 (m, 4H), 2.61 (m, 4H), 2.34 (s, 3H). ESI-MS: m/z 449.10 [M+H]+.
WORKUP
后处理
- customThe reaction tube was sealed
- customThe product was purified by column chromatography (5% CH3OH/CH2Cl2)