反应详情

A mixture of tert-butyl 2-(6-chloro-5-methylpyridin-3-yl) acetate 86-6 (7.8 g, 32 mmol) and TFA (32 mL) in DCM (32 mL) was stirred at room temperature for 3 hours. The solution was adjusted to pH around 12 by sodium carbonate and extracted with dichloromethane. The aqueous phase was acidified to pH 3 by 1N HCl aqueous solution and stirred for 15 minutes. The suspension was extracted with dichloromethane (100 mL X3). The combined organic phases were washed with water and brine, dried over Na2SO4 and then dried to give 2-(6-chloro-5-methylpyridin-3-yl)acetic acid 86-7 as pale yellow solid. MS m/z 186.1 (M+1); 1H NMR 400 MHz (CD3Cl) δ 8.17(d, 1H, J=2.0 Hz), 7.55(d, 1H, J=2.0 Hz), 3.63(s, 2H), 2.38(s, 3H).

1. extractionextracted with dichloromethane
2. stirringstirred for 15 minutes
3. extractionThe suspension was extracted with dichloromethane (100 mL X3)
4. washThe combined organic phases were washed with water and brine
5. dry with materialdried over Na2SO4
6. customdried