Reaktion #576408
ord-93c2e3cc1941461180df679fb132fe9a
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling to room temperature
- 2Waschenwashed with water (3 times)
- 3TrocknenThe organic layer was dried over Na2SO4
- 4Sonstigeevaporated in vacuo
- 5SonstigeThe 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).