反応 #1509590

反応方程式

methylamine

3-chlorocarbonyl-5-nitro-benzoic acid ethyl ester

→

title compound

N-Methyl-5-nitro-isophthalamic acid ethyl ester

溶媒

THF

THF

反応条件

後処理

1. 1
   ろ過filtered
2. 2
   濃縮The filtrate was concentrated in vacuum
3. 3
   その他the solid recrystallised from diethyl ether

実験手順

To a 2M solution of methylamine in THF (256 ml) at −20° C. was added a pre-cooled solution of 3-chlorocarbonyl-5-nitro-benzoic acid ethyl ester (60 g) in THF (500 ml) dropwise. This was stirred for 20 min and then filtered. The filtrate was concentrated in vacuum and the solid recrystallised from diethyl ether to give the title compound (22.5 g) as a solid. An oxalyl chloride solution in DCM (63 ml, 2M), was added with DMF (5 ml). The reaction was stirred for 2 h and then concentrated in vacuum. The residue was triturated with toluene and again concentrated in vacuum leaving the title compound (60 g). Rt=1.53 min (method D).

出典