HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenylacetylene → HCID 19090127, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenylacetylene | HCID 10821 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 1-Methyl-4-iodo-1H-pyrazole | HCID 2734773 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Catalyst | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| Solvent | Diisopropylamine | HCID 7912 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 19090127 | HCID 19090127 | — |
Reaction Steps
To a solution of 1-methyl-4-iodopyrazole (208 g, 1 mol) and phenylacetylene (112 g, 1.1 mol) in diisopropylamine (2 l) are added, under nitrogen, copperiodide (2 g), triphenylphosphine (0.1 g) and bis-(triphenylphosphine) palladiumdichloride (0.5 g). The mixture is kept during 3 hours at ca. +35° C. and then heated for 1 hour at +90° C. The cooled reaction mixture is diluted with ethyl acetate and filtrated. Concentration of the filtrate and distillation yields the title compound: b.p. 116°-118° C./0.3 mbar, m.p. 70°-72° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05300521 |
| Source dataset | uspto-grants-1994_04 |
| ORD ID | ord-1b52132531514c289474cd56ed19290d |
| Source note | uspto-grants-1994_04 |