Reaktion #576408

ord-93c2e3cc1941461180df679fb132fe9a

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    TemperaturAfter cooling to room temperature
  2. 2
    Waschenwashed with water (3 times)
  3. 3
    TrocknenThe organic layer was dried over Na2SO4
  4. 4
    Sonstigeevaporated in vacuo
  5. 5
    SonstigeThe residue was purified by preparative chromatography

Vorschrift

A mixture of ethyl-2-methylthiazole 4-carboxylate (500 mg, 2.9 mmol), N-bromosuccinimide (877 mg, 4.9 mmol), and benzoyl peroxide (5-10 mg ) in 1,2-DCE (3 mL) was heated at 70° C. for 85 h. After cooling to room temperature, DCM (10 ml) was added and washed with water (3 times). The organic layer was dried over Na2SO4 and evaporated in vacuo. The residue was purified by preparative chromatography to yield the above-titled compound (58 mg). 1H NMR (CDCl3): 8.23 (1H, s), 4.77 (2H, s), 4.43 (2H, q), 1.42 (3H, t).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06977267B2uspto-grants-2005_12