Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178467665 | HCID 178467665 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22241628 | HCID 22241628 | 47.6% |
Reaction Steps
To a solution of the product from Step A (1.2 g, 4.28 mmol) in DMF (10 ml) was added iodomethane (0.53 ml, 8.6 mmol) and potassium carbonate (1.2 g, 8.6 mmol); this mixture was stirred for 16 h at 70° C. After adding water (15 ml) and ethyl acetate (15 ml) to the reaction mixture, the aqueous layer was separated and extracted with ethyl acetate (3×20 ml). The combined extracts were washed with brine, dried (MgSO4), and evaporated to a residue which was puified by chromatography (silica, ethyl acetate/hexane, 1:1) to give a viscous oil (0.6 g): APCl/LCMS m/z 295 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07005443B1 |
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| Source dataset | uspto-grants-2006_02 |
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| ORD ID | ord-9dd87f58283a4d8eade06778c3505f70 |
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| Source note | uspto-grants-2006_02 |
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