反应详情

A solution of 9.1 parts of 5-chloro-2,3-dihydro-4-benzofuranamine [described in J. Het. Chem., 17(6) 1333 (1980)], 9.6 parts of N-bromosuccinimide and 130.5 parts of benzene was stirred for 1 hour at reflux temperature. The solvent was evaporated and the residue was dissolved in 387.4 parts of trichloromethane. The solution was washed with water (2×200 parts). The organic layer was dried, filtered and evaporated. The residue was purified by column chromatography (silica gel; C6H14 /CH2Cl2 50:50). The eluent of the desired fraction was evaporated, yielding 11.8 parts (87.9%) of 7-bromo-5-chloro-2,3-dihydro-4-benzofuranamine (interm. 8).

1. temperatureat reflux temperature
2. customThe solvent was evaporated
3. dissolutionthe residue was dissolved in 387.4 parts of trichloromethane
4. washThe solution was washed with water (2×200 parts)
5. customThe organic layer was dried
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by column chromatography (silica gel; C6H14 /CH2Cl2 50:50)
9. customThe eluent of the desired fraction was evaporated