Reaktionsgleichung
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5].N([O-])=O.[Na+].C([O-])(=O)C.[Na+].[N-:27]=[N+:28]=[N-].[Na+]>C(O)(=O)C.Cl.O>[N:1]([C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5])=[N+:27]=[N-:28]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
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.
Aufarbeitung
- filtrationThe turbid solution is clarified by filtration
- customThe reaction product which has precipitated
- filtrationis filtered off
- washwashed with water until neutral
- dry with materialAfter drying over potassium hydroxide/calcium chloride in a desiccator
Quellen und Nachweise
- ORD-Eintrag
- ord-74449a8db68b4211b700be4941ae260f
- Quelldatensatz
- uspto-grants-1976_03
- Patentnummer
- US03943145
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