反应详情

2-Iodo-5-nitroanisole (5.58 g, 20.0 mmol), Pd2(dba)3 (0.025 eq, 457 mg), Xantphos (0.05 eq, 578 mg), Hunigs Base (1 eq, 3.48 ml) and sodium methanethiolate (1 eq, 1.40 g) were dissolved in THF. The mixture was heated to reflux overnight. Upon cooling the mixture was filtered through celite. The filtrate was concentrated in vacuo. The residue was purified by flash chromatography (4:1 Hexanes/Ethyl Acetate) to give 2-methoxy-1-methylsulfanyl-4-nitro-benzene (2.72 g, 68.3%) as a yellow crystalline solid.

1. temperatureThe mixture was heated
2. temperatureto reflux overnight
3. temperatureUpon cooling the mixture
4. filtrationwas filtered through celite
5. concentrationThe filtrate was concentrated in vacuo
6. customThe residue was purified by flash chromatography (4:1 Hexanes/Ethyl Acetate)