Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 178437194 | HCID 178437194 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178463863 | HCID 178463863 | 63.9% |
Reaction Steps
A mixture of 2 g (8.1 mmol) 2-amino-1-chloro-3-(1H-imidazol-4-yl)butane dihydrochloride, 1.3 g (16.2 mmol) sodium acetate and 100 ml 10% acetic acid, are hydrogenated over 0.5 g 10% palladium on activated carbon for 10 days at 10 bar and ambient temperature. The catalyst is removed by filtration and the filtrate brought to pH 1 by addition of concentrated hydrochloric acid. After evaporation the oily residue is dissolved in dry ethanol and inorganic material is removed by filtration. By addition of petrolether the title compound crystallizes as dihydrochloride. Recrystallization from methanol/acetonitrile yields 0.72 g (40.4%) [3-(1H-imidazol-4yl)but-2-yl]amine.2HCl.0.25 methanol as colorless crystals, melting point: 249°-254° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05034539 |
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| Source dataset | uspto-grants-1991_07 |
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| ORD ID | ord-fcaba1e92da14567bfbe4c38dbb7c4dc |
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| Source note | uspto-grants-1991_07 |
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