反应详情

A solution of the 3-methyl-2-(2-methyl-1-propenyl)benzoic acid ethyl ester (290) (3 g-0.014 mol) in MeOH (50 mL) is treated with 2N NaOH (10 mL) and refluxed for 6 h. The solvent is removed in vacuo and the residue diluted with water (75 mL). The aqueous phase is extracted with EtOAc (30 mL) and then separated and acidified to pH 2-3 with concentrated HCl. The solid precipitated is extracted into EtOAc (3×50 mL). The extracts are washed with water (2×30 mL) and brine (2×30 mL), and dried over MgSO4 and concentrated in vacuo to give the product as white solid (2.0 g, 75%).

1. temperaturerefluxed for 6 h
2. customThe solvent is removed in vacuo
3. additionthe residue diluted with water (75 mL)
4. extractionThe aqueous phase is extracted with EtOAc (30 mL)
5. customseparated
6. customThe solid precipitated
7. extractionis extracted into EtOAc (3×50 mL)
8. washThe extracts are washed with water (2×30 mL) and brine (2×30 mL)
9. dry with materialdried over MgSO4
10. concentrationconcentrated in vacuo