Reaktion #86544
ord-92f53ceabd6d4381b252a49e4df22896
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling
- 2FiltrationThe mixture was filtered
- 3Sonstigethe collected precipitate was air-dried
- 4Sonstigeto give crude product which
Vorschrift
A mixture of polyphosphoric acid (73.8 g, 677 mmol), 1,3-thiazol-2-amine (12.3 g, 123 mmol), and methyl 4-bromo-3-oxopentanoate (34.8 g, 166 mmol) was stirred at 110° C. overnight. After cooling, an ice-cold 10% aq. NaOH solution was slowly added to adjust the pH to 7. The mixture was filtered, and the collected precipitate was air-dried to give crude product which was directly used in next step. LCMS calculated for C8H8BrN2OS (M+H)+: m/z=259.0. Found: 259.0.