反应 #68408

反应方程式

1-iodo-4-methoxy-2-nitrobenzene

3-methyl-1-butyne

→

title compound

4-Methoxy-1-(3-methylbut-1-ynyl)-2-nitrobenzene

溶剂

Et3N

DMF

反应条件

后处理

1. 1
   浓缩was concentrated
2. 2
   workup.ADDITIONThe resulting mixture was diluted with EtOAc
3. 3
   洗涤washed with H2O, brine
4. 4
   干燥dried over Na2SO4
5. 5
   浓缩concentrated in vacuo
6. 6
   其他The residue was purified by chromatography on silica gel (0→15% EtOAc-hexanes)

实验过程

To a solution of 1-iodo-4-methoxy-2-nitrobenzene (Aldrich, 10 g, 35.8 mmol) in Et3N (60 ml) and DMF (6 ml) was added CuI (34 mg, 0.18 mmol), Pd(PPh3)2Cl2 (126 mg, 0.18 mmol), and 3-methyl-1-butyne (5.0 ml, 73.5 mmol). The mixture was stirred at room temperature for 16 h and was concentrated. The resulting mixture was diluted with EtOAc, washed with H2O, brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→15% EtOAc-hexanes) to yield the title compound as a brown oil.

来源