Sulfuric Acid → 1312454-85-5
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:14])/[CH:11]=N/O)[CH:5]=[C:6]([F:8])[CH:7]=1.[OH:15]S(O)(=O)=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:5]([C:11](=[O:15])[C:10](=[O:14])[NH:9]2)=[C:6]([F:8])[CH:7]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
(E)-N-(3-bromo-5-fluorophenyl)-2-(hydroxyimino)acetamide (6.13 g, 23.6 mmol) was slowly added to a solution of conc. H2SO4 (30 mL) in an ice bath. The temperature of the reaction mixture was maintained below 50° C. After completion of the addition, the solution was heated to 90° C. for 1 h. After it was cooled to rt, the mixture was poured into ice-water and stirred vigorously for 1 h. The insoluble solid was filtered and washed with water, dried under vacuum to provide 7.4 g of crude product, which was used into the next step without further purification. MS (ESI): 242, 244 (MH−).
Aufarbeitung
- temperatureThe temperature of the reaction mixture was maintained below 50° C
- additionAfter completion of the addition
- temperatureAfter it was cooled to rt
- filtrationThe insoluble solid was filtered
- washwashed with water
- customdried under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-f1dc82d4ff814c8d979a94c482203825
- Quelldatensatz
- uspto-grants-2014_07
- Patentnummer
- US08772301B2
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