反应详情

温度

60 °C

4-chloro-3-nitropyridine (1.1 eq) was added to a solution of 3-methylpiperidine-3-carboxylic acid (1 eq) and DIEA (3 eq) in iPrOH (0.1 M). The reaction mixture was heated in a 60° C. oil bath for 3 h then concentrated in vacuo. The crude residue was diluted with EtOAc and washed with 1.0 N NaOH. The combined aqueous washes were acidified to pH=4 with 1.0 N HCl and extracted with CH2Cl2. The combined organic phases were dried over anhydrous MgSO4, filtered, and concentrated in vacuo to give 3-methyl-(3-nitropyridin-4-yl)piperidine-3-carboxylic acid. LC/MS (m/z): 266.2 (MH+).

1. concentrationthen concentrated in vacuo
2. additionThe crude residue was diluted with EtOAc
3. washwashed with 1.0 N NaOH
4. extractionextracted with CH2Cl2
5. dry with materialThe combined organic phases were dried over anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo