HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 3-Bromo-1-methyl-1,2-dihydropyridin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178517701 | HCID 178517701 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-Bromo-1-methyl-1,2-dihydropyridin-2-one | HCID 13024025 | — |
Reaction Steps
To a solution of 3-bromo-pyridin-2-ol (10 g, 57.47 mmol) in DMF (100 ml) at 0° C. was added NaH (60%, 2.52 g, 63.22 mmol) portionwise under argon. After 30 min methyl iodide (4.29 ml, 68.97 mmol) was added dropwise and the reaction mixture was stirred for 15 h at RT. The mixture was diluted with ethyl acetate (100 ml), washed with water (2×200 ml) and brine (100 ml), dried over Na2SO4, and evaporated under reduced pressure. The crude product was used without further purification in step 21.5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08378092B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-cc017c8edf8b434d88e70efb2c5a9dc2 |
| Source note | uspto-grants-2013_02 |