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With sulfuric acid; nitric acid; In acetic acid; at 70.0℃; for 0.25h;
L-METHOXY-3, 5-DIMETHYLBENZENE (4.12 g, 30 mmoles) was dissolved in acetic acid (20 ml). To this solution was added dropwise a mixture of nitric acid (1.26 ml, 30 mmoles) and concentrated sulfuric acid (1.9 ML, 35 mmoles). The mixture was heated at 70 C for 15 minutes. After cooling, water was added and the mixture was extracted with dichloromethane. The organic extract was dry and evaporated. The resulting residue was purified by column chromatography (30% heptane in CH2CI2). Yield: 1.91 g of intermediate 34 (35%).
35%
With sulfuric acid; nitric acid; In acetic acid; at 70.0℃; for 0.25h;
Example A3; a) Preparation of intermediate 5; l-methoxy-3,5-dimethylbenzene (4.12g, 30 mmoles) was dissolved in acetic acid (20 ml). To this solution was added dropwise a mixture of nitric acid fuming (1.26 ml, 30 mmoles) and concentrated sulfuric acid (1.9 ml, 35 mmoles). The mixture was heated at 70 C for 15 minutes. After cooling, water was added and the mixture was extracted with dichloromethane. The organic extract was dried and evaporated. The resulting residue was purified by column chromatography (30% heptane in CH2CI2). Yield : 1.91g (35%) of intermediate 5 (CI-MS : 182 [M+H]+).
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