反应详情

A suspension of 4-(4-chlorobenzoyl)-3,5-dichlorobenzyl bromide (3.2 g, 8.5 mmol) and potassium azide (1.3 g, 16 mmol) in ethanol (32 ml) was refluxed 5 hours, cooled, and filtered. The precipitate was washed once with ethanol and the combined filtrate and wash were evaporated under vacuum. The residue was triturated with diethyl ether (50 ml) and filtered. The filtrate was evaporated under vacuum to provide 2.92 g (100%) of 4-(4-chlorobenzoyl)-3,5-dichlorobenzyl azide, m.p. 50°-55° C.

1. temperaturewas refluxed 5 hours
2. temperaturecooled
3. filtrationfiltered
4. washThe precipitate was washed once with ethanol
5. washthe combined filtrate and wash
6. customwere evaporated under vacuum
7. customThe residue was triturated with diethyl ether (50 ml)
8. filtrationfiltered
9. customThe filtrate was evaporated under vacuum