HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 21180499, compound → HCID 9861789, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 21180499 | HCID 21180499 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9861789 | HCID 9861789 | 43% |
Reaction Steps
A solution of 3-[2-(3,4-dichloro-phenyl)-3H-imidazol-4-yl]-benzonitrile (4.1 g, 13 mmol), in THF (130 ml) was slowly added to an ice-cooled mixture of lithium aluminum hydride (0.99 g, 26 mmol) in THF (130 ml). The mixture was stirred for 30 min. at r.t., then saturated Seignette-salt solution (5 ml) was added slowly and stirring was continued for 30 min. The precipitate was filtered and the organic phase evaporated and chromatographed over SiO2 with CH2Cl2—CH3OH—NH4OH (140:10:1) to obtain 3-[2-(3,4-dichloro-phenyl)-3H-imidazol-4-yl]-benzylamine (1.77 g, 43%) as a foam. The hydrochloride salt was then prepared which was crystallized to an off-white solid. Mp. >250° C. (MeOH/Et2O), MS: m/e=318 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06265426B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-897d5a7b1d7f4f069b08c4b6f6e812de |
| Source note | uspto-grants-2001_07 |