HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methyl-3-butyn-2-ol → HCID 20481568, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methyl-3-butyn-2-ol | HCID 8258 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 10757956 | HCID 10757956 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 20481568 | HCID 20481568 | 99.3% |
Reaction Steps
To 142 g (0.45 mole) of 1-(4'-iodophenoxy)-2-diethylaminoethane, 1.2 liters of triethylamine and 37.8 g (0.45 mole) of 3-methyl-1-butin-3-ol are added, under nitrogen, 3.4 g of the palladium complex PdCl2 [P(C6H5)3 ]2 and 1.9 g of copper(I) iodide. After the exothermic reaction has subsided, the reaction mixture is stirred for 15 hours at room temperature, then filtered, and the solution is evaporated in vacuo to dryness. The oily residue crystallises immediately. The product is dried in vacuo at 40° C., affording 123 g (99%) of 1-(3-hydroxy-3-methyl-1-butyn-1-yl)-4-(2-diethylaminoethoxy)benzene with a melting point of 64° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04412856 |
| Source dataset | uspto-grants-1983_11 |
| ORD ID | ord-d1d264575a6347048634997002fe44aa |
| Source note | uspto-grants-1983_11 |