HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 58236582, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 58236629 | HCID 58236629 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58236582 | HCID 58236582 | 88.2% |
Reaction Steps
To a solution of 365 (0.49 g, 0.76 mmol) in MeOH (100 mL) was added iron dust (0.43 g, 7.6 mmol) and ammonium chloride (0.12 g, 2.3 mmol) in water (5 mL). The resulting mixture was heated to reflux for 4 h, then cooled, filtered through a celite pad and concentrated. The residue was partitioned between dichloromethane and water; the organic phase was collected, washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography (eluent 2% MeOH in EtOAc) to give 366 (0.41 g, 88% yield). LRMS (M+H): 612.6
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08729268B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-0be7b15571104332842455025880145c |
| Source note | uspto-grants-2014_05 |