反应详情

温度

5 °C

A 6N aqueous sodium hydroxide solution (17 ml) was added dropwise to a stirred solution of 4-chloro-2-fluoro-5-methoxycarbonyloxy-1-nitrobenzene (J. Med. Chem., 1999, 42, 5369; 25 g) in methanol (200 ml) which was cooled to 5° C. The reaction mixture was stirred at ambient temperature for 30 minutes. A 12N aqueous hydrochloric acid solution (8.5 ml) was added and the mixture was evaporated. The residue was partitioned between methylene chloride and water. The organic layer was washed with brine, dried over magnesium sulphate and evaporated to give 4-chloro-2-fluoro-5-hydroxy-1-nitrobenzene (18.5 g); NMR Spectrum: (CDCl3) 5.8 (br s, 1H), 7.35 (d, 1H), 7.75 (d, 1H).

1. customthe mixture was evaporated
2. customThe residue was partitioned between methylene chloride and water
3. washThe organic layer was washed with brine
4. dry with materialdried over magnesium sulphate
5. customevaporated