反应详情

温度

70 °C

To a suspension suspension of Pyridine-2-carboxylic acid (2-acetyl-5-methoxy-phenyl)-amide (2.90 g, 10.7 mmol) in THF (50 mL) was added t-BuOK/THF (1M, 24 mL, 24 mmol). The reaction mixture was heated at 70° C. for 3 h and stirred overnite. The solvent was removed the in vacuo. Cold water was added to the residue and adjusted pH to 4.6 with aqueous 1.0 N HCl, filtered. The solid residue was purified over a Biotage 65M column (MeOH/CH2Cl2: 0 to 15%) to provide the product (2.26 g, 84%): LC-MS (retention time: 1.19, Method D), MS m/z 253 (M++1).

1. customThe solvent was removed the in vacuo
2. additionCold water was added to the residue
3. filtrationfiltered
4. customThe solid residue was purified over a Biotage 65M column (MeOH/CH2Cl2: 0 to 15%)