反应详情

温度

65 °C

2,4-Di-tert-butyl-6-(4,7-dibromo-benzotriazol-2-yl)-phenol (Monomer T1) (1.0 g, 2.08 mmol) and potassium carbonate (0.431 g, 96% GC purity, 3.12 mmol) were mixed in anhydrous DMF (20 mL) in a round-bottomed 100-mL flask. The flask was capped with a rubber septum and purged with nitrogen for 0.5 h. The mixture was heated to 65° C. and iodomethane (0.591 g, 4.16 mmol) was added. The mixture was stirred at 60-65° C. for 1 h. The flask was cooled to room temperature. DCM (20 mL) and water (20 mL) were added and the organic phase was separated and the aqueous phase extracted with DCM (20 mL). All the organic phases were combined and washed with water (3×20 mL) and brine (20 mL). The solution was dried over magnesium sulfate and filtered. The filtrate was evaporated to dryness with a rotary evaporator. The product was crystallized from DCM/hexanes and filtered. Purity: 99% (GC). Yield: 34%.

1. customThe flask was capped with a rubber septum
2. custompurged with nitrogen for 0.5 h
3. temperatureThe flask was cooled to room temperature
4. customthe organic phase was separated
5. extractionthe aqueous phase extracted with DCM (20 mL)
6. washwashed with water (3×20 mL) and brine (20 mL)
7. dry with materialThe solution was dried over magnesium sulfate
8. filtrationfiltered
9. customThe filtrate was evaporated to dryness with a rotary evaporator
10. customThe product was crystallized from DCM/hexanes
11. filtrationfiltered