HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 2-(2,5-Dimethyl-1H-pyrrol-1-yl)-6-ethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 2-(2,5-Dimethyl-1H-pyrrol-1-yl)-6-methylpyridine | HCID 793156 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(2,5-Dimethyl-1H-pyrrol-1-yl)-6-ethylpyridine | HCID 13398304 | 60% |
Reaction Conditions
| Temperature | -30 °C |
|---|
Reaction Steps
To a solution of the product from Example 2a (6.82 g, 36.6 mmol) in 75 mL of dry THF cooled to 40° C. under a N2 atmosphere was added dropwise n-BuLi as a 2.5M solution in hexanes (16 mL, 40 mmol). The resulting solution was stirred at low temperature for thirty minutes then treated with CH3I (2.4 mL, 38.6 mmol). On completion of the addition the mixture was allowed to warm to −30° C. and after 20 min to room temperature. The reaction was subsequently quenched by pouring into brine solution, the product isolated by extraction with EtOAc. Dried over MgSO4, filtered and concentration under vacuum. Purified by silica gel column chromatography eluting with EtOAc/hexane gave the title compound (4.42 g, 60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338605B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-f8f8f12a40b64ba285499e46cd80ebe4 |
| Source note | uspto-grants-2012_12 |