反应详情

4N aqueous sodium hydroxide solution (17 ml) was added to an ice cooled suspension of methyl 3,4-dimethoxy-2-methanesulfonyloxy-6-nitrobenzoate (1.74 g, 0.0052 mol) in dioxane (9 ml) and the resulting orange solution stirred for 1 hour. The reaction mixture was acidified with 2N aqueous hydrochloric acid and extracted with dichloromethane (2×50 ml). The combined organic extracts were dried (MgSO4), filtered and evaporated under reduced pressure to give the subtitle compound as a white solid (1.23 g, 92%). MS m/z 275 (MNH4)+. 1H-NMR (CDCl3): δ=3.92 (9H, m), 6.86 (1H, s), 9.66 (1H, s).

1. temperaturecooled
2. extractionextracted with dichloromethane (2×50 ml)
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. filtrationfiltered
5. customevaporated under reduced pressure