反応 #1153522

反応方程式

3-fluoro-4-nitrobenzoic acid

N-methyl-2,4-dichlorobenzylamine

sodium carbonate

→

3-(N-methyl-2,4-dichlorobenzylamino)-4-nitrobenzoic acid

収率 44.3%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   抽出The reaction mixture was extracted
2. 2
   workup.STIRRINGwith stirring
3. 3
   その他The organic layer was separated
4. 4
   濃縮concentrated
5. 5
   workup.ADDITIONmethanol was added to the resulting residue
6. 6
   その他After removal of an insoluble material
7. 7
   その他the solvent was evaporated
8. 8
   その他The resulting residue was purified by silica-gel column chromatography

実験手順

A solution of 10 ml N,N-dimethylformamide containing 3-fluoro-4-nitrobenzoic acid (1.00 g), N-methyl-2,4-dichlorobenzylamine (1.54 g) and sodium carbonate (1.15 g) was stirred at 100° C. for 14 hours. The reaction mixture was extracted using water and ethyl acetate with stirring. The organic layer was separated and concentrated, and then methanol was added to the resulting residue. After removal of an insoluble material, the solvent was evaporated. The resulting residue was purified by silica-gel column chromatography to give 0.85 g of 3-(N-methyl-2,4-dichlorobenzylamino)-4-nitrobenzoic acid.

出典