反应详情

To a stirred solution of methyl 2-ethoxy-2′-methyl-1,1′-biphenyl-4-carboxylate (11 g, 40.6 mmol) in a mixture of THF (100 mL) and water (10 mL) was added lithium hydroxide (6.82 g, 162.7 mmol) in portions. After 24 hours at RT, the reaction mixture was evaporated and the residue was taken up with water. The aqueous layer was acidified with a concentrated aqueous solution of HCl and extracted with EtOAc. The organic layer was washed with brine, dried (Na2SO4) and concentrated under vacuum affording of the title compound as pale yellow solid (9.7 g, 93%). LC/MS (Method B): 255.0 (M−H)−. 1H-NMR (DMSO-d6, 400 MHz) δ 13.02 (br s, 1H), 7.57 (m, 2H), 7.18-7.25 (m, 4H), 7.09 (d, 1H), 4.05 (q, 2H), 2.05 (s, 3H), 1.18 (t, 3H).

1. customthe reaction mixture was evaporated
2. extractionextracted with EtOAc
3. washThe organic layer was washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under vacuum