HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57846996, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 11698468 | HCID 11698468 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57846996 | HCID 57846996 | 63% |
Reaction Steps
To a solution of the compound (119 mg, 0.252 mmol) synthesized in Example 81 in DMF (1 ml) was added sodium hydride (60% in oil, 12.1 mg, 0.30 mmol) under ice-cooling, and the mixture was stirred for 1 hr. Methyl iodide (0.0187 ml, 0.30 mmol) was added dropwise and the mixture was stirred overnight at room temperature. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous MgSO4, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography using silica gel and eluted with hexane-ethyl acetate (5:95, v/v) to give the title compound (76.5 mg, 63%) as an amorphous form.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973163B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-cc9324f70dc048a0b256c9253682deae |
| Source note | uspto-grants-2011_07 |