HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 44242881, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178527301 | HCID 178527301 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 44242881 | HCID 44242881 | 43% |
Reaction Steps
A solution of 5-(4-benzylpiperazin-1-yl)-3-(phenylsulfonyl)-1H-indazole (433 mg, 1.00 mmol) in THF at room temperature is treated with NaH (80 mg, 60% in mineral oil, 2.00 mmol), stirred for 0.5 h, treated with methyl iodide (142 mg, 1.00 mmol), stirred for 16 h, and diluted with water and EtOAc. The organic phase is separated, dried over MgSO4, and concentrated in vacuo. The resultant residue is chromatographed (SiO2, 90:10 EtOAc:hexanes as eluent) to afford the title compound as a white solid, 190 mg (43% yield), mp 195-197° C., identified by mass spectral and NMR analyses.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07560470B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-ed231522cff142d892a9444259b4743a |
| Source note | uspto-grants-2009_07 |