HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 12647522, compound → HCID 11195816, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 12647522 | HCID 12647522 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11195816 | HCID 11195816 | 66.6% |
Reaction Steps
To a solution of methylmagnesium bromide (3.0 M in diethyl ether (12.0 mL, 36.0 mmol)) and copper(I) iodide (6.86 g, 36.0 mmol) in THF (100 mL) was added 48.1 (6.73 g, 30.0 mmol) at room temperature. The resulting mixture was refluxed for 4 hours. The mixture was then cooled in an ice-bath, quenched with aqueous NH4Cl (200 mL), extracted with ether, concentrated, and purified by silica gel column chromatography to give 48.2 (4.8 g, 66% yield). MS ESI (pos.) M/E: 241 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450522B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-e3b5e43dea144517944eee22c2a24923 |
| Source note | uspto-grants-2013_05 |