反应详情

温度

60 °C

A solution of methyl 2′-methyl-2-(trifluoromethyl)biphenyl-4-carboxylate (5 g; 16.99 mmol; 1 eq.) in EtOH (150 mL) at RT was treated with sodium hydroxide (10.2 mL; 5 M; 51 mmol; 3 eq.). The reaction mixture was stirred at 60° C. for 2 hours. The reaction mixture was concentrated to give a brown solid which was taken up in water (300 mL) and the aqueous phase was washed twice with EtOAc. The aqueous phase was acidified with HCl cc to pH 2, then it was concentrated until precipitation (half of the volume). The suspension was filtered affording the title compound as a beige solid. 1H NMR (DMSO-d6, 300 MHz) δ 13.55 (br s, 1H), 8.31 (s, 1H), 8.26-8.23 (d, J=7.90 Hz, 1H), 7.51-7.48 (d, J=7.90 Hz 1H), 7.37-7.12 (m, 4H), 1.99 (s, 3H). LC/MS (Method A): 278.9 (M−H)−. HPLC (Method A) Rt 4.57 min (Purity: 98.7%).

1. concentrationThe reaction mixture was concentrated
2. customto give a brown solid which
3. washthe aqueous phase was washed twice with EtOAc
4. concentrationit was concentrated until precipitation (half of the volume)
5. filtrationThe suspension was filtered