反应详情

A stirred suspension of 4-(4-chlorobenzoyl)-3-chlorobenzyl bromide (1.60 g, 4.65 mmol) and potassium azide (0.715 g, 8.81 mmol) in ethanol (15 ml) was refluxed 5 hours, cooled to ambient temperature, and stirred 16 hours. The solids were filtered and washed twice with ethanol. The combined filtrate and washes were evaporated under vacuum, diluted with diethyl ether (40 ml), filtered, and evaporated under vacuum to provide 1.51 g (106% of theory) of 4-(4-chlorobenzoyl)-3-chlorobenzyl azide, m.p. 33°-33.5° C., suitable for subsequent reaction.

1. temperaturewas refluxed 5 hours
2. filtrationThe solids were filtered
3. washwashed twice with ethanol
4. customThe combined filtrate and washes were evaporated under vacuum
5. additiondiluted with diethyl ether (40 ml)
6. filtrationfiltered
7. customevaporated under vacuum