反应详情

温度

60 °C

2.3 ml of thionyl chloride are added dropwise to an ice-cooled solution of 5.40 g 5-tert-butyl-2-methoxy-3-nitro-benzoic acid in 50 ml of methanol. The cooling bath is removed and the solution is heated to 60° C. The solution is stirred overnight at 60° C. and then cooled to ambient temperature. The solution is evaporated down completely and the residue is mixed with water. The aqueous mixture is extracted with ethyl acetate, and the combined extracts are dried (MgSO4). The solvent is removed, and the residue is chromatographed on silica gel with cyclohexane/ethyl acetate (98:2→60:40).

1. customThe cooling bath is removed
2. temperaturecooled to ambient temperature
3. customThe solution is evaporated down completely
4. additionthe residue is mixed with water
5. extractionThe aqueous mixture is extracted with ethyl acetate
6. dry with materialthe combined extracts are dried (MgSO4)
7. customThe solvent is removed
8. customthe residue is chromatographed on silica gel with cyclohexane/ethyl acetate (98:2→60:40)