反应详情

温度

60 °C

A mixture of 2-aminobenzamide (681 mg, 5.0 mmol), 2,4,5-trichloropyrimidine (2.75 g, 15 mmol, 3 equiv.) and concentrated HCl (aq) (1.72 mL, 20 mmol, 4 equiv.) in 2-propanol (100 mL) is heated at 60° C. for 12 h. The 2-propanol solvent is removed in vacuo. The resulting residue is neutralized to approximately pH=7 by adding 1 N NaOH (aq) followed by partition between EtOAc and water. Upon partition between EtOAc and water, a significant amount of precipitate is produced. This precipitate is collected by vacuum filtration and washed with small amounts of EtOAc and water, providing the product 2-(2,5-dichloropyrimidin-4-ylamino)benzamide; ESMS m/z 283.0 (M+H+).

1. customThe 2-propanol solvent is removed in vacuo
2. additionby adding 1 N NaOH (aq)
3. customby partition between EtOAc and water
4. customUpon partition between EtOAc and water
5. customa significant amount of precipitate is produced
6. filtrationThis precipitate is collected by vacuum filtration
7. washwashed with small amounts of EtOAc and water