반응 #68408

반응 방정식

1-iodo-4-methoxy-2-nitrobenzene

3-methyl-1-butyne

→

title compound

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

용매

Et3N

DMF

반응 조건

후처리

1. 1
   농축was concentrated
2. 2
   workup.ADDITIONThe resulting mixture was diluted with EtOAc
3. 3
   세척washed with H2O, brine
4. 4
   건조dried over Na2SO4
5. 5
   농축concentrated in vacuo
6. 6
   기타The residue was purified by chromatography on silica gel (0→15% EtOAc-hexanes)

실험 절차

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.

출처