Reaktion #617166

ord-bb88ab245fa3415391d1da0ce529f151

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe precipitate was filtered
  2. 2
    Waschenwashed with ether
  3. 3
    Filtrationthe precipitate was filtered
  4. 4
    Waschenwashed with ether
  5. 5
    Sonstigedried in air

Vorschrift

The crude N′-[5-(2-chloro-benzoyl)-thiazol-2-yl]-N,N-dimethyl-formamidine was dissolved in 10% HCl (150 mL) and heated to 70° C. for 4 hours. The precipitate was filtered, washed with ether, and then suspended in a 10% sodium carbonate solution (250 mL). The suspension was stirred for 1 hour and the precipitate was filtered, washed with ether, and dried in air to give (2-amino-thiazol-5-yl)-(2-chloro-phenyl)-methanone as a brown solid (8.5 g, 36 mmol, 55% from 1-(2-chloro-phenyl)-ethanone). 1H NMR (400 MHz, DMSO-d6) δ 7.27 (s, 1H), 7.41-7.58 (m, 4H), 8.37 (s, 2H). ESI-MS m/z calc. 238.0, found; 239.3 (M+1)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09351962B2uspto-grants-2016_05