HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 1-Methyl-5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 68003854 | HCID 68003854 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Methyl-5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one | HCID 58562865 | — |
Reaction Steps
To a suspension of sodium hydride (27 mg, 1.07 mmol, 95%) in THF under argon was added 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one (135 mg, 0.60 mmol, prepared in the Example 12 Step E). After stirring 1 hour at room temperature, Methyl iodide (0.07 mL, 1.12 mmol) was added dropwise and the reaction stirred at room temperature overnight. The reaction mixture was poured onto saturated NaHCO3 and extracted with ethyl acetate. The organic layer was concentrated in vacuo and the residue purified by flash chromatography (silica gel, 0-100% ethyl acetate/DCM).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062048B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-45e09f18d26048f38dfa67758f5d6bd2 |
| Source note | uspto-grants-2015_06 |