反应详情

温度

0 °C

0.1 g of 2-amino-5-chloro-N-(1-cyclopropylethyl)benzamide was dissolved in 3 ml of N,N-dimethylformamide and cooled to 0° C. 0.02 g of sodium hydride was added, followed by stirring for one hour, and 0.09 g of bromine was added, followed by stirring for 2 hours. The reaction liquid was added to a 1 M-HCl aqueous solution, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 1/1) to obtain 0.08 g of the pale yellow desired produce (melting point: 177° C.).

1. stirringby stirring for 2 hours
2. customThe reaction liquid
3. extractionfollowed by extraction with ethyl acetate
4. washThe organic layer was washed with a saturated sodium chloride aqueous solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 1/1)
8. customto obtain 0.08 g of the pale
9. customyellow desired produce (melting point: 177° C.)