HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 67305534, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Lithium perchlorate | HCID 23665649 | — |
| Reactant | HCID 57659372 | HCID 57659372 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67305534 | HCID 67305534 | — |
Reaction Steps
Sodium hydride (60% dispersed in oil, 58 mg) was washed with anhydrous 2,2,4-trimethylpentane and suspended in anhydrous THF. Lithium perchlorate (78 mg, 0.73 mmol) was added to the suspension at 0° C., followed by (3aR,9bS)-tert-butyl 2-oxo-1,2,3,3a,4,9b-hexahydrospiro[benzo[g]indole-5,4′-piperidine]-1′-carboxylate (142 mg, 0.4 mmol) in THF (10 ml) at 0° C. After 15 min, methyl iodide (0.04 ml, 0.6 mmol) was added. The reaction mixture was stirred at room temperature for 1 h then heated under reflux for 1 h. Concentration gave the title compound. LC-MS: m/e=371.6 (M+), 315.5 (M−tBu+1, 100%). Rt=3.12 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973162B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-a73912cff30249ccb9fe6b49f129f1d0 |
| Source note | uspto-grants-2011_07 |