HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Nitrophenyl isocyanate → HCID 66589697, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Nitrophenyl isocyanate | HCID 76835 | — |
| Reactant | 3-(5-(aminomethyl)-1-oxo-2,3-dihydro-1H-isoindol-2-yl)piperidine-2,6-dione hydrochloride | HCID 66589525 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66589697 | HCID 66589697 | 39% |
Reaction Steps
To a stirred mixture of 3-(5-aminomethyl-1-oxo-1,3-dihydro-isoindol-2-yl)-piperidine-2,6-dione hydrochloride (0.74 g, 2.00 mmol) and 3-nitropheny isocyanate (0.33 g, 2.00 mmol) in acetonitrile (20 mL) was added TEA (0.56 mL, 4.00 mmol) at RT under nitrogen. After 12 hrs, the solid was filtered and purified by preparative HPLC (gradient: CH3CN/H2O: 15/85 for 5 min, to 100/0 in 10 min, 100/0 for 5 min). After evaporation of the solvent, the residue was triturated in ether (20 mL) for 1 hr. The product was then isolated by filtration and dried in vacuo to give 1-((2-(2,6-dioxopiperidin-3-yl)-1-oxoisoindolin-5-yl)methyl)-3-(3-nitrophenyl)urea as a yellow solid (0.34 g, 39% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227954B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-4a667ee4fd8b4c72a414ca720bffca4e |
| Source note | uspto-grants-2016_01 |