HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 67106673, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178429126 | HCID 178429126 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67106673 | HCID 67106673 | 66.1% |
Reaction Steps
To a stirred suspension of sodium hydride (0.2 g of 50% in mineral oil, 4.2 mmol) in THF was added (4,4-dimethyl-oxazolidin-2-ylidene)-(4-nitro-phenyl)-amine (1 g, 4.25 mmol), stirred for 30 min at r.t., followed by addition of iodomethane (0.71 g, 5.0 mmol). After a further 6 hours at r.t. the reaction was quenched with water and extracted with ethyl acetate. The extracts were washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give a residue which was purified by column chromatography over silica gel (60-120 mesh) using 15% ethyl acetate/petroleum ether as eluent to give (4-nitro phenyl)-(3,4,4-trimethyl-oxazolidin-2-ylidene)-amine (0.7 g, 66%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08604029B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-4e2fea706e1e4040a7d34aad9f494954 |
| Source note | uspto-grants-2013_12 |