反应详情

温度

167.5 °C

A mixture of 4-methylanisole (200 g, 1.64 mol), benzyl alcohol (40.0 g, 0.37 mol) and p-toluenesulfonic acid monohydrate (8.0 g, 0.042 mol) was stirred at 160 to 175° C. for two hours while eliminating water generated by the reaction. After excess 4-methylanisole was distilled off under reduced pressure (inner temperature, 132° C./25 mmHg (3.3 kPa), the residue was dissolved in toluene (50 ml) and then the organic layer was successively washed with water (20 ml), 10% aqueous caustic soda (20 ml) and water (20 ml). After the washed organic layer was concentrated, the residue was distilled under reduced pressure to collect a component fractionated at boiling point of 120-138° C. at 0.7 mmHg (0.09 kPa) as a main fraction (52.75 g, 67.2%). The component was analyzed by NMR to identify 2.7:1 mixture of 2-benzyl-4-methylanisole and 3-benzyl-4-methylanisole.

1. customgenerated by the reaction
2. distillationAfter excess 4-methylanisole was distilled off under reduced pressure (inner temperature, 132° C./25 mmHg (3.3 kPa)
3. dissolutionthe residue was dissolved in toluene (50 ml)
4. washthe organic layer was successively washed with water (20 ml), 10% aqueous caustic soda (20 ml) and water (20 ml)
5. concentrationAfter the washed organic layer was concentrated
6. distillationthe residue was distilled under reduced pressure
7. customto collect a component
8. addition2.7:1 mixture of 2-benzyl-4-methylanisole and 3-benzyl-4-methylanisole