Reaktionsgleichung
[N:1]1([CH:6]([C:8]2[CH:13]=[CH:12][C:11]([NH:14][CH:15]=[O:16])=[CH:10][CH:9]=2)[CH3:7])[CH:5]=[CH:4][N:3]=[CH:2]1.S(=O)(=O)(O)O.[N+:22]([O-])([O-:24])=[O:23].[K+].[OH-].[NH4+]>>[N:1]1([CH:6]([C:8]2[CH:13]=[CH:12][C:11]([NH:14][CH:15]=[O:16])=[C:10]([N+:22]([O-:24])=[O:23])[CH:9]=2)[CH3:7])[CH:5]=[CH:4][N:3]=[CH:2]1Komponenten
Versuchsvorschrift
(a-4) To a cooled and stirred solution of 13 parts of N-[4-[1-(1H-imidazol-1-yl)ethyl]phenyl]formamide in 92 parts of concentrated sulfuric acid was added portionwise 6.1 parts of potassium nitrate at a temperature between -5° to -10° C. Upon completion, stirring was continued for 1.50 hour at 0° C. The reaction mixture was poured into crushed ice. The whole was treated with ammonium hydroxide at 0°~-10° C. The product was extracted three times with 195 parts of dichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from 48 parts of 2-propanol. The product was filtered off and dried, yielding 5.4 parts (34.6%) of N-[4-[1-(1H-imidazol-1-yl)-ethyl]-2-nitrophenyl]formamide; mp. 158° C. (int. 116).
Aufarbeitung
- temperature(a-4) To a cooled
- additionThe reaction mixture was poured
- custominto crushed ice
- extractionThe product was extracted three times with 195 parts of dichloromethane
- customThe extract was dried
- filtrationfiltered
- customevaporated
- customThe residue was crystallized from 48 parts of 2-propanol
- filtrationThe product was filtered off
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-d5a74b4b641149dcab3796bec92c7aeb
- Quelldatensatz
- uspto-grants-1989_08
- Patentnummer
- US04859684
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