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 5h. 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-bydroxybenzoate 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 5h
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
10. customto afford 9.65 g (90%) of methyl 3-tert-butyl-4-bydroxybenzoate as a white crystalline solid, m.p. 144-145° C.