反应详情

10 G (0.04 mol) of 2-amino-5-chloro-2'-fluorobenzophenone are dissolved in a mixture of 40 ml of glacial acetic acid and 10 ml of concentrated hydrochloric acid and diazotised with 10 ml (0.04 mol) of 4 M sodium nitrite solution. The mixture is then diluted with 200 ml of ice-cold water and neutralised by addition of 16.3 g (0.12 mol) of crystalline sodium acetate. The turbid solution is clarified by filtration using active charcoal and a solution of 8.5 g (0.13 mol) of sodium azide in 100 ml of water is then added. The reaction product which has precipitated is filtered off and washed with water until neutral. After drying over potassium hydroxide/calcium chloride in a desiccator, 2-azido-5-chloro-2'-fluorobenzophenone of decomposition point 90°C is obtained.

1. filtrationThe turbid solution is clarified by filtration
2. customThe reaction product which has precipitated
3. filtrationis filtered off
4. washwashed with water until neutral
5. dry with materialAfter drying over potassium hydroxide/calcium chloride in a desiccator