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
- 105 °C
PROCEDURE
实验过程
A microwave tube is charged with 30 mg (0.123 mmol) of 8-Bromo-2-chloro-quinoxaline, 26.4 mg (0.123 mmol) of 3,4,5-trimethoxyphenylboronic acid, 40 mg (0.370 mmol) of Na2CO3 and 4.4 mg (0.0037 mmol) of Pd(PPh3)4. After several cycles of vacuum/purge with argon, 1.5 ml of dry DMF are added. The reaction mixture is then heated tot 105° C. for 15 h. After cooling, the yellow suspension is poured onto de-ionized water and filtered. After drying under H.V. at 50° C., the residue is purified by chromatography (silicagel, hexane:EtOAc=100=>1:1) to afford the title compound as a yellow solid, Rt=1.294 min (Acquity HPLC BEH C18, 2.1×50 mm, 1.7 micron, detection 215 nM, 0.1 min 2% CH3CN in H2O, 2% to 100% CH3CN in H2O in 1.5 min, 0.4 min 100% CH3CN+0.1% TFA, flow rate 1.0 ml/min); MS: 375 (M)+.
WORKUP
后处理
- customAfter several cycles of vacuum/purge with argon, 1.5 ml of dry DMF
- additionare added
- temperatureAfter cooling
- additionthe yellow suspension is poured onto de-ionized water
- filtrationfiltered
- customAfter drying under H.V
- customat 50° C., the residue is purified by chromatography (silicagel, hexane:EtOAc=100=>1:1)