HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68999229, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 69002133 | HCID 69002133 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 68999229 | HCID 68999229 | 20% |
Reaction Steps
To a solution of (E)-2-{2-[2-(1H-indazol-3-yl)vinyl]phenyl}-4-nitro-2,3-dihydroisoindol-1-one (54 mg, 0.14 mmol) obtained in Step 1 in ethanol/water (2/1, 3.3 mL), ammonium chloride (40 mg, 0.75 mmol) and iron (38 mg, 0.68 mmol) were added, followed by heating under reflux for 4.0 hours under nitrogen atomosphere. The reaction mixture was added with water, extracted with ethyl acetate and the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform to chloroform/methanol=90/10) and crystallized from hexane/ethyl acetate (1/1) to obtain Compound 216 (10 mg, 20%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07605272B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-dc2526e15da14bbd9046f3f62904b214 |
| Source note | uspto-grants-2009_10 |