反应详情

Phosphoryl chloride (12.7 ml) was dropwise added to N,N-dimethylformamide (70 ml), and the mixture was stirred for 30 minutes at ambient temperature. A solution of N-benzyl-3,5-dichloro-N-methylaniline (7.26 g) in N,N-dimethylformamide (30 ml) was dropwise added thereto, and the mixture was stirred for 30 minutes at ambient temperature and then for 30 minutes at 50° C. The reaction mixture was neutralized with 1N aqueous sodium hydroxide solution and extracted with ethyl acetate. The organic solution was washed with water and brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by a flash chromatography (ethyl acetate:n-hexane=1:6, V/V) to give N-benzyl-3,5-dichloro-4-formyl-N-methylaniline (5.70 g).

1. stirringthe mixture was stirred for 30 minutes at ambient temperature
2. waitfor 30 minutes at 50° C
3. extractionextracted with ethyl acetate
4. washThe organic solution was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by a flash chromatography (ethyl acetate:n-hexane=1:6, V/V)