반응 #1933457
ord-4df33a92f03240109a1b97594008ec40
반응 조건
온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타the solvent was removed under reduced pressure
- 2workup.ADDITIONthe residue was diluted with ethyl acetate
- 3세척washed with 1 N aqueous solution of sodium hydroxide, water
- 4건조dried over sodium sulfate
- 5기타The crude oil (7 g) was purified by column chromatography (silica gel 230-400 mesh; 10/0 to 4/1 hexanes/EtOAc as eluent)
실험 절차
To a solution of isatoic anhydride (4.00 g, 24.0 mmol) in N,N-dimethyl formamide (80 mL) under nitrogen atmosphere was added 4-sec-butylaniline (3.66 g, 24.0 mmol). The reaction mixture was heated at 80° C. for 24 hours, then the solvent was removed under reduced pressure and the residue was diluted with ethyl acetate, washed with 1 N aqueous solution of sodium hydroxide, water, and dried over sodium sulfate. The crude oil (7 g) was purified by column chromatography (silica gel 230-400 mesh; 10/0 to 4/1 hexanes/EtOAc as eluent) to give pure 2-amino-N-(4-sec-butylphenyl)-benzamide as a brown solid. Yield: 1.8 g (27.3%).