反应详情

To a solution of 4′-cyano-6-methyl-biphenyl-3-carboxylic acid methyl ester 2 (2.56 g, 10.3 mmol) in 1,4-dioxane-H2O (1:1 mixture, 20 ml) is added NaOH (1.22 g, 30.2 mmol)). The reaction is stirred at ambient temperature for 24 hours. To this mixture is added aqueous HCl (1 N, 36 ml) and it is then extracted with ethyl acetate (40 ml×3). The organic layers are combined, dried over anhydrous Na2SO4. The solver is removed. The solid obtained is washed with small amount of acetonitrile and air dried to give 4′-cyano-6-methyl-biphenyl-3-carboxylic acid 3: 1H NMR (DMSO-d6) δ 7.94 (d, 2 H, J=8.0 Hz), 7.84 (dd, 1 H, J1=8.4 Hz, J2=1.2 Hz), 7.75 (d, 1 H, J=1.2 Hz), 7.61 (d, 2 H, J=8.0 Hz), 7.48 (d, 1 H, J=8.4 Hz), 2.29 (s, 3H); LC-MS m/z 238.1 (M+1).

1. extractionis then extracted with ethyl acetate (40 ml×3)
2. dry with materialdried over anhydrous Na2SO4
3. customThe solver is removed
4. customThe solid obtained
5. washis washed with small amount of acetonitrile and air
6. customdried