HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 178525122, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | Benzyl 4-formylpiperidine-1-carboxylate | HCID 2776272 | — |
| Reactant | 1-(3,4-Dichlorophenyl)-2-pyridin-4-yl-ethane-1,2-dione | HCID 15454860 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178525122 | HCID 178525122 | — |
Reaction Steps
1-(3,4-Dichlorophenyl)-2-pyridin-4-yl-ethane-1,2-dione (2.8 g, 10 mmol), 4-formylpiperidine-1-carboxylic acid benzyl ester (2.47 g, 10 mmol) and ammonium acetate (7.7 g, 100 mmol) were dissolved in acetic acid (65 mL) and heated to reflux for 2.5 hour and allowed to cool to ambient temperature. The reaction mixture was then poured over an ammonium hydroxide (100 mL) and ice mixture. This aqueous layer was extracted with ethyl acetate (3×200 mL) and the organic layers were combined, washed with brine (100 mL), dried over anhydrous magnesium sulfate, filtered and concentrated at reduced pressure. The resulting oil was chromatographed on silica gel eluting with 97:3 dichloromethane:methanol to give the imidazole as a foam (2.3 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06083949 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-9e0f9496d146482c8bcf1ead5a032c9b |
| Source note | uspto-grants-2000_07 |