HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178515418, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | Ethyl 2-Cyano-3-(5,6,7,8-tetrahydro-1-isoquinolylamino)-acrylate | HCID 70583309 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178515418 | HCID 178515418 | 19% |
Reaction Steps
Aluminum chloride (2.05 g., 0.0154 mole) was added to cold (-30° C.) tetrahydrofuran (75 ml.). Sodium azide was added and the mixture heated under reflux for 40 minutes. Ethyl 2-cyano-3-(5,6,7,8-tetrahydro-1-isoquinolylamino)-acrylate (3.33 g., 0.0123 mole) was added and the mixture heated under reflux for 20 hours. The cooled mixture was diluted with water (100 ml.) and acidified with concentrated hydrochloric acid. The precipitate was collected, washed with water, dried and recrystallized from 2-methoxyethanol to give the title compound (0.625 g., 19%), m.p. 290°-292° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04209620 |
| Source dataset | uspto-grants-1980_06 |
| ORD ID | ord-9b70d8fc53ab47ddb5fffd815045b648 |
| Source note | uspto-grants-1980_06 |