HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178468760, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 15654659 | HCID 15654659 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178468760 | HCID 178468760 | 52% |
Reaction Steps
A mixture of ethyl 1-[(2'-cyanobiphenyl-4-yl)methyl]-2-isopropylbenzimidazole-7-carboxylate (2.12 g), sodium azide (3.9 g) and ammonium chloride (3.2 g) in DMF (15 ml) was stirred for 5 days at 110°-120 C. To the reaction mixture was added water (150 ml), which was made acidic (pH 3-4) with dilute hydrochloric acid, followed by extraction with ethyl acetate. The organic layer was washed with water, dried and concentrated to dryness. The concentrate was crystallized from ethanol to afford colorless prisms (1.2 g, 52%), m.p. 144°-146° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05128356 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-0c3ada84a2c44cb5b2d76f8c7bfbb010 |
| Source note | uspto-grants-1992_07 |