反应详情

Dissolve homophthalic acid (22.2 g, 0.123 mmol) in tetrahydrofuran (250 mL) and add dropwise at room temperature to a slurry of lithium aluminum hydride (15.5 g, 0.407 mol) in tetrahydrofuran (500 mL). Heat at reflux for 18 hours, cool in an ice bath and carefully add, by dropwise addition, water (16 mL), followed by 50% sodium hydroxide (16 mL). Remove the ice bath, add water slowly with stirring and stir until the gray precipitate turns white and evolution of gas ceases. Filter, wash solids with methylene chloride, dry (MgSO4) and evaporate the solvent in vacuo to give 2-(2-hydroxymethyl-phenyl)-ethanol as a viscous oil (18.4 g, 98%).

1. temperatureHeat
2. temperatureat reflux for 18 hours
3. temperaturecool in an ice bath
4. customRemove the ice bath
5. additionadd water slowly
6. stirringstir until the gray precipitate
7. filtrationFilter
8. washwash solids with methylene chloride
9. dry with materialdry (MgSO4)
10. customevaporate the solvent in vacuo