反应详情

10.0 g of 3-fluoro-4-methylsulfanylnitrobenzene prepared in the above example 1, 0.1 eq of Pd/C (5 wt %), 4 eq of amonium formate were dissolved in THF/MeOH (1:1) and refluxed for 3 hours. The solid, which was not dissolved in the solution, was filtered away, and the filtrate was distilled under reduced pressure to obtain oily compound, which was dissolved again in 80 ml of ethyl acetate. Solid amonium formate which was not dissolved in the solution, was filtered away, and the filtrate was distilled under reduced pressure to obtain oily filtrate, which was purified by column chromatography (ethyl acetate:n-Hexane=1:3) to give 6.04 g of the title compound as a yellow solid (yield 88%).

1. temperaturerefluxed for 3 hours
2. dissolutionThe solid, which was not dissolved in the solution
3. filtrationwas filtered away
4. distillationthe filtrate was distilled under reduced pressure
5. customto obtain oily compound, which
6. filtrationwas filtered away
7. distillationthe filtrate was distilled under reduced pressure
8. customto obtain oily filtrate, which
9. customwas purified by column chromatography (ethyl acetate:n-Hexane=1:3)