Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 16726205 | HCID 16726205 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59301263 | HCID 59301263 | 34% |
Reaction Steps
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%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07714099B2 |
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| Source dataset | uspto-grants-2010_05 |
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| ORD ID | ord-05e5485519f94e268824500adacac145 |
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| Source note | uspto-grants-2010_05 |
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