HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 17952492, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 17952493 | HCID 17952493 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 17952492 | HCID 17952492 | 6.3% |
Reaction Steps
A solution of 2-(1,3-diethyl-2-oxo-2,3-dihydro-1H-benzoimidazol-5-yl)-4-pyridin-3-yl-1-m-tolyl-butane-1,4-dione (600 mg, 1.13 mmol) and ammonium acetate (871 mg, 11.3 mmol) in acetic acid (3.77 mL) was heated at 110° C. for 4 hours. The reaction was then poured over a mixture of ice and NH4OH and stirred for 5 minutes. The aqueous mixture was extracted with EtOAc (3×10 mL). The organics were combined, washed with brine, dried over sodium sulfate, and concentrated in vacuo to give a orange oil. The oil was purified by flash chromatography using a gradient of Et2O to 50% EtOAc/Et2O, affording 30 mg of the title compound. MS (M+1)=423.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07056918B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-0cbef19f229944c5ad9472f26c893bf0 |
| Source note | uspto-grants-2006_06 |