反应详情

温度

60 °C

To a solution of methyl 2-(methoxymethyl)-2′-methylbiphenyl-4-carboxylate obtained in step 3 (40 g; 147.97 mmol) in EtOH (1200 mL) was added NaOH (88.78 mL; 5 M; 443.90 mmol) after which the mixture was heated at 60° C. for one hour. Reaction mixture was cooled to room temperature 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 to give the title compound as a yellow solid (35.1 g, 92%). 1H NMR (DMSO-d6) δ 12.99 (br s, 1H), 8.09 (s, 1H), 7.92-7.89 (m, 1H), 7.33-7.22 (m, 4H), 7.10-7.08 (m, 1H), 4.11 (m, 2H), 3.18 (s, 3H), 1.99 (s, 3H). HPLC (Method A) Rt 4.52 min (Purity: 96.4%). LC/MS (Method B): 255.2 (M−H)−.

1. customReaction mixture
2. temperaturewas cooled to room temperature
3. concentrationconcentrated under vacuum
4. customto give a yellow solid
5. washthe aqueous phase was washed with EtOAc
6. extractionextracted with EtOAc