Reacción #1869219
ord-f3955082ebdf49f99c8913127af764d7
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
80°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1TemperaturaThe resulting mixture was cooled
- 2FiltraciónSolid (bis-alkylated product) was filtered off
- 3Extracciónwas extracted with ether
- 4Otrothe organics were dried
- 5Concentraciónconcentrated in vacuo
- 6OtroPurification by RPHPLC (Xterra, gradient 95-5%, ammonia (0.2% aq.) in acetonitrile)
Procedimiento
A mixture of 4,6-dichlororesorcinol (2 g), potassium carbonate (1.54 g) and methyl bromoacetate (1.71 g) in DMF (10 ml) was heated at 80° C. for 24 h. The resulting mixture was cooled and water (200 ml) added. Solid (bis-alkylated product) was filtered off, then the aqueous was acidified with aq. HCl, which was extracted with ether and the organics were dried and concentrated in vacuo. Purification by RPHPLC (Xterra, gradient 95-5%, ammonia (0.2% aq.) in acetonitrile) gave the subtitle compound (0.65 g) as a solid.