HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68931533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 68936688 | HCID 68936688 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68931533 | HCID 68931533 | 33% |
Reaction Steps
To a solution of the compound (0.060 g) obtained in Example 642 in DMF (1 mL) was added sodium hydride (0.005 g) and the mixture was stirred for 10 min. Methyl iodide (0.020 mL) was added at 0° C. and the mixture was stirred at room temperature. To the reaction mixture was added water, and the resultant product was extracted with ethyl acetate. The organic layer was washed with brine and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH Chromatorex) (solvent gradient; 30→70% ethyl acetate/hexane) to give the title compound (0.020 g, 33%) 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-74277777865045dc8f72a09524b1d792 |
| Source note | uspto-grants-2013_06 |