反应详情

温度

-78 °C

N-methyl-N-methyloxy-2-amino-4-chlorobenzamide (3.6 g) and N-tert-butoxycarbonyl-3-bromobenzylamine (5.5 g) were dissolved in tetrahydrofuran (50 ml). The solution was cooled to −78° C., to which was added dropwise, while stirring, a hexane solution of n-butyl lithium (1.6 mol/L, 60 ml) over 40 minutes. To the reaction mixture was added water, which was subjected to extraction with ethyl acetate (150 ml). The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off. The residue was purified by means of a silica gel column chromatography to give 2-amino-3-tert-butoxycarbonylaminomethyl-4-chlorobenzophenone as a yellow oily product (2.3 g).

1. additionwas added dropwise
2. extractionwas subjected to extraction with ethyl acetate (150 ml)
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was distilled off
6. customThe residue was purified by means of a silica gel column chromatography