HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 59577945, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 59577874 | HCID 59577874 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59577945 | HCID 59577945 | — |
Reaction Steps
To NaH (0.04 g, 55% suspension in oil, washed with pentane) was added at RT and under an argon atmosphere and at RT 4-[8-(2-chloro-benzenesulfonyl)-1-oxo-2,8-diaza-spiro[4.5]dec-2-yl]-N-isopropyl-benzamide (0.04 g), product of example 160), in THF (4 ml). The reaction mixture was stirred 1 hour at RT, then MeI (0.232 g) was added and stirring was continued overnight at RT until the conversion was complete. The reaction mixture was made acidic with 1M HCl (one drop) and stirred for one minute. The solvent was removed in vacuo, the residue adsorbed on silica gel and chromtographed over silica gel (eluent: AcoEt/CH2Cl2, gradient from 0 to 30%) to give the desired product as off-white solid. MS (ESI): 504.1 MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08329904B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-44b939c539ab4c73be5e98068f6216d1 |
| Source note | uspto-grants-2012_12 |