HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 59239867, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 59239858 | HCID 59239858 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59239867 | HCID 59239867 | — |
Reaction Steps
tert-Butyl 2-acetyl-1-[4-(ethoxycarbonyl)phenyl]hydrazinecarboxylate (606 mg) was dissolved in DMF (10 ml), and methyl iodide (0.14 ml) and then sodium hydride (60%, 83 mg) were added at 0° C. The mixture was stirred at room temperature for 3 hr. The reaction mixture was diluted with ethyl acetate, and washed with water and then saturated brine. The organic layer was dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1 (volume ratio)→1:1 (volume ratio)), and further recrystallized from ethyl acetate-hexane to give the title compound (608 mg) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989445B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-7823687a4cae432a821201126569e5c9 |
| Source note | uspto-grants-2011_08 |