反应详情

A mixture of 4-chloro-2-chloromethyl-1-nitro-benzene (85 g, 0.41 mol), glycine ethyl ester hydrochloride (70 g, 0.50 mol) and triethylamine (121.4 ml, 0.8665 mol) in ethanol (1000 ml) was heated at reflux for 8 h. The solvent was evaporated and the residue was triturated in warm tert-butyl methyl ether. The ammonium salts were removed by filtration and the filtrate was concentrated in vacuo to give the title compound (111 g, 99%) as an amorphous brown solid which was used in the next step without purification. MS m/e: 273 (M+H+).

1. temperaturewas heated
2. temperatureat reflux for 8 h
3. customThe solvent was evaporated
4. customthe residue was triturated in warm tert-butyl methyl ether
5. customThe ammonium salts were removed by filtration
6. concentrationthe filtrate was concentrated in vacuo