反应 #1269894

反应方程式

4-chloro-2-chloromethyl-1-nitro-benzene

glycine ethyl ester hydrochloride

triethylamine

→

title compound

收率 99.3%

(5-Chloro-2-nitro-benzylamino)-acetic acid ethyl ester

收率 99.3%

溶剂

ethanol

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for 8 h
3. 3
   其他The solvent was evaporated
4. 4
   其他the residue was triturated in warm tert-butyl methyl ether
5. 5
   其他The ammonium salts were removed by filtration
6. 6
   浓缩the filtrate was concentrated in vacuo

实验过程

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+).

来源