反应详情

To a stirring solution of 2-amino-5-chloropyridine (3.7 g, 29 mmol) and pyridine (7.3 mL, 90 mmol) in dichloromethane (200 mL) was added 2-nitrobenzoyl chloride (5.7 g, 30 mmol). After stirring for 4 h, the solvents were removed in vacuo and the residue was partitioned between ethyl acetate and water. The layers were separated and the organic phase was washed again with water and once with brine, then dried with MgSO4, filtered and partially concentrated in vacuo. The precipitate was filtered, washed with diethyl ether and dried in vacuo to give 6.4 g (79%) of an off-white solid.

1. customthe solvents were removed in vacuo
2. customthe residue was partitioned between ethyl acetate and water
3. customThe layers were separated
4. washthe organic phase was washed again with water and once with brine
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. concentrationpartially concentrated in vacuo
8. filtrationThe precipitate was filtered
9. washwashed with diethyl ether
10. customdried in vacuo