反应详情

温度

95 °C

3-Methoxy-2-methyl-phenol was prepared according to published procedure: J. Org. Chem. 55, 5, 1990, 1469. To a solution of 2.0 g (50 mmol) NaOH and 2-methylresorcinol (6.2 g, 50 mmol) in water (50 mL), dimethylsulfate (4.8 mL, 50 mmol) was added at 95° C. over 30 min, then reaction was stirred for 2 h at 95° C. After cooling to RT, the reaction mixture was poured into aqueous NaOH (8.0 g in 200 ml H2O). Extracted with Et2O (2×100 mL). The aqueous phase was acidified with 5 N aq. HCl, extracted with Et2O (2×100 mL), extracts were dried over Na2SO4 and evaporated. The residue was purified on SiO2 (200 g) column, hexane—EtOAc (0 to 20%). Yield 3.37 g (24.0 mmol, 49%), colorless oil.

1. customreaction
2. temperatureAfter cooling to RT
3. extractionExtracted with Et2O (2×100 mL)
4. extractionextracted with Et2O (2×100 mL), extracts
5. dry with materialwere dried over Na2SO4
6. customevaporated
7. customThe residue was purified on SiO2 (200 g) column, hexane—EtOAc (0 to 20%)