HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 21698922, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 21698918 | HCID 21698918 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21698922 | HCID 21698922 | 42.9% |
Reaction Steps
2-[7-Fluoro-5-nitro-2H-1,4-benzoxazine-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (1.3 g) was dissolved in anhydrous dimethylformamide (15 ml) and was slowly added to a stirred suspension of sodium hydride (0.11 g) in dimethylformamide (15 ml) under ice cooling. Solution was stirred for 0.5 hr followed by the addition of methyl iodide (2.03 g). After stirring for 2 hr at ambient temperature, solution was added to ice-water and product was isolated by partitioning with ethyl acetate. Purification by column chromatography on silica gel in hexane-ethyl acetate (3:1) afforded the title compound (0.58 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06294503B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-bbc0f1b4967647df8f4fd2bf0956e5c6 |
| Source note | uspto-grants-2001_09 |