反应详情

温度

60 °C

To a stirred solution of 2-amino-N-[2-(2,4-dichlorophenyl)ethyl]-4-nitrobenzamide (1.0 g, 2.82 mmol) in toluene (30 mL) was added a 1.9 M solution of phosgene in toluene (4.5 mL, 8.5 mmol). The reaction mixture was heated to 60° C. and stirred for 4 hours. The solvent was removed under reduced pressure and CH2Cl2 was added to the residue. The precipitate was collected via vacuum filtration and washed with CH2Cl2 to give the product (0.92 g, 86% yield) as a white solid. HPLC retention time: 3.28 min; Method A; LRMS (ESI) m/z 378 (M−1).

1. customThe solvent was removed under reduced pressure and CH2Cl2
2. additionwas added to the residue
3. filtrationThe precipitate was collected via vacuum filtration
4. washwashed with CH2Cl2