تفاعل #1269894
ord-cb2452808eb148b98e3f17211b0064ca
معادلة التفاعل
4-chloro-2-chloromethyl-1-nitro-benzene
glycine ethyl ester hydrochloride
triethylamine
→
title compound
المردود 99.3%
(5-Chloro-2-nitro-benzylamino)-acetic acid ethyl ester
المردود 99.3%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas heated
- 2درجة الحرارةat reflux for 8 h
- 3أخرىThe solvent was evaporated
- 4أخرىthe residue was triturated in warm tert-butyl methyl ether
- 5أخرىThe ammonium salts were removed by filtration
- 6تركيزthe filtrate was concentrated in vacuo
الإجراء التجريبي
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+).