Reaktion #86544

ord-92f53ceabd6d4381b252a49e4df22896

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    FiltrationThe mixture was filtered
  3. 3
    Sonstigethe collected precipitate was air-dried
  4. 4
    Sonstigeto 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434746B2uspto-grants-2016_09