反应详情

温度

60 °C

To a solution of methyl 4-bromo-3-(methoxymethyl)benzoate (Intermediate 28, step 2), (7 g; 27.02 mmol) in EtOH (210 mL) was added NaOH (16.21 mL; 5 M; 81.05 mmol). The resulting reaction mixture was heated at 60° C. for one hour. It was then cooled to RT and concentrated under vacuum to give a yellow solid. Water was added and the aqueous phase was washed with EtOAc. The aqueous phase was then acidified with HCl (1 M) and extracted with EtOAc. Organic phase was dried over MgSO4, filtered and concentrated under vacuum to give the title compound as a yellow solid (5.81 g, 87%). 1H NMR (DMSO-d6, 300 MHz) 13.19 (br s, 1H), 8 (m, 1H), 7.77-7.76 (m, 2H), 4.49 (s, 2H), 3.40 (s, 3H). LC/MS (Method B): 245.0 (M−H)−. HPLC (Method A) Rt 3.63 min (purity: 97.4%).

1. customThe resulting reaction mixture
2. temperatureIt was then cooled to RT
3. concentrationconcentrated under vacuum
4. customto give a yellow solid
5. washthe aqueous phase was washed with EtOAc
6. extractionextracted with EtOAc
7. dry with materialOrganic phase was dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated under vacuum