HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 87212338, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 58123826 | HCID 58123826 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 87212338 | HCID 87212338 | — |
Reaction Steps
Methyl iodide (80 μL) is added to a mixture of (2R,6S)-2,2,2-trifluoro-1-(10-hydroxy-6,11,11-trimethyl-9-nitro-1,2,5,6-tetrahydro-4H-2,6-methano-benzo[d]azocin-3-yl)-ethanone (0.40 g) and potassium carbonate (0.17 g) in dimethylformamide (5 mL). The mixture is stirred at room temperature overnight, before another portion of methyl iodide (80 μL) and potassium carbonate (0.16 g) are added. The mixture is stirred for another 6 h at room temperature. Then, water and ethyl acetate are added, the organic phase is separated, and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with brine and dried (Na2SO4). The solvent is evaporated to give the crude product that is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859580B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-512b15e37a124f43b0d5c724367d5352 |
| Source note | uspto-grants-2014_10 |