Reaktion #1880043

ord-c368e0a839684f7b84c75961fa20ac31

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: US07078420B2uspto-grants-2006_07