反应详情

Combine 4-(3-Fluoro-5-nitro-phenylsulfanyl)-1-methyl-piperidine (preparation 75, 0.31 g, 1.15 mmol), iron dust (0.21 g, 3.79 mmol), methanol (10 mL) and aqueous 1M hydrochloric acid (0.35 mL, 0.35 mmol), stir and heat at reflux. After 20 h, cool to ambient temperature and concentrate. Partition residue between ethyl acetate (50 mL) and 1M sodium hydroxide (20 mL). Separate the organic layer, dry over sodium sulfate, filter and concentrate. Purify residue by silica gel flash chromatography eluting with 10% (2M NH3/methanol)/methylene dichloride to obtain 0.11 g (40%) of the title compound: mass spectrum (electrospray): m/z=241.1 (M+1).

1. temperatureheat
2. temperatureat reflux
3. concentrationconcentrate
4. customSeparate the organic layer
5. dry with materialdry over sodium sulfate
6. filtrationfilter
7. concentrationconcentrate
8. washPurify residue by silica gel flash chromatography eluting with 10% (2M NH3/methanol)/methylene dichloride