反应详情

温度

100 °C

To a solution of methyl 2,2′-dimethyl-1,1′-biphenyl-4-carboxylate, prepared in Step 1 (15 g, 62.2 mmol) in THF (100 mL) was added 10% sodium hydroxide (100 mL) and the mixture was heated to 100° C. overnight. THF was removed under reduced pressure and the aqueous residue was washed with EtOAc. The aqueous layer was then acidified with 3N HCl to pH 2-3 and extracted with DCM. The organic phase was washed with water and dried over sodium sulfate and concentrated under reduced pressure to obtain get the title compound as a white solid (13.5 g, 95%). 1H NMR: (DMSO-d6, 400 MHz) δ 12.89 (bs, 1H), 7.89 (s, 1H), 7.82-7.80 (d, 1H), 7.32-7.23 (m, 3H), 7.19-7.11 (d, 1H), 7.07-7.05 (d, 1H), 2.04 (s, 3H), 1.98 (s, 3H). LC/MS (Method A): 227.0 (M+H)+. HPLC (Method B), Rt: 4.1 min (purity: 99.6%).

1. customTHF was removed under reduced pressure
2. washthe aqueous residue was washed with EtOAc
3. extractionextracted with DCM
4. washThe organic phase was washed with water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customto obtain