HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178515926, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | trans-3-(4-oxo-4H-1-benzopyran-3-yl)-acrylonitrile | HCID 12330012 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178515926 | HCID 178515926 | — |
Reaction Steps
Under stirring, 4.6 parts of anhydrous aluminum chloride are added to 100 volume parts of dry tetrahydrofuran, followed by the addition of 3.11 parts of trans-3-(4-oxo-4H-1-benzopyran-3-yl)-acrylonitrile and 4.5 parts of sodium azide. The whole mixture is refluxed for 28 hours and, then, 35 volume parts of 15 weight% hydrochloric acid are added to the resulting mixture, followed by distilling off tetrahydrofuran under reduced pressure. The resulting residue is recovered by filtration and recrystallized from methanol, dimethylformamide-water and, then, from methanol. This procedure yields trans-1-(4-oxo-4H-1-benzopyran-3-yl)-2-(1H-tetrazol-5-yl) ethylene as light-yellow needles. Melting point: 254.5°-255° C.(decomp. with foaming).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04151180 |
| Source dataset | uspto-grants-1979_04 |
| ORD ID | ord-d08d479268884998901ac9c819611fbe |
| Source note | uspto-grants-1979_04 |