反应详情

To a 500 mL 3-necked flask equipped with a magnetic stirrer, a nitrogen inlet, and a condenser were added 10.0 g of 3-tert-butyl-4-hydroxybenzoic acid (ICN Biomedicals. Inc., Aurora, Ohio 44202), and 200 mL of MeOH. The solution was acidified by bubbling HCl gas through for 5 min. and was then heated at reflux for 5 h. The solution was cooled to RT and concentrated in vacuo to dryness. The resulting solid was dissolved in EtOAc. The solution was washed three times with 5% aqueous NaHCO3, dried over anhydrous MgSO4 and concentrated to dryness to afford 9.65 g (90%) of methyl-3-tert-butyl-4-hydroxybenzoate as a white crystalline solid, m.p. 144-145° C.

1. customTo a 500 mL 3-necked flask equipped with a magnetic stirrer, a nitrogen inlet, and a condenser
2. customby bubbling HCl gas through for 5 min.
3. temperaturewas then heated
4. temperatureat reflux for 5 h
5. concentrationconcentrated in vacuo to dryness
6. dissolutionThe resulting solid was dissolved in EtOAc
7. washThe solution was washed three times with 5% aqueous NaHCO3
8. dry with materialdried over anhydrous MgSO4
9. concentrationconcentrated to dryness