HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68928964, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 68930226 | HCID 68930226 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68928964 | HCID 68928964 | 54% |
Reaction Steps
To a solution of the compound obtained in Example 459 (100 mg) in DMF (3 mL) was added sodium tert-butoxide (25.3 mg) at 0° C., and the mixture was stirred for 5 min. Then, methyl iodide (16.5 μL) was added, and the mixture was stirred at room temperature for 14 hr. The reaction mixture was poured into water, and the resultant product was extracted with ethyl acetate. The organic layer was washed with water and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent gradient; 0→12% methanol/ethyl acetate) to give the title compound (55 mg, 54%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08470816B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-e0a7741688a942499071c2f3080aa087 |
| Source note | uspto-grants-2013_06 |