HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Difluoro-3-nitrobenzene → Nitrobenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Difluoro-3-nitrobenzene | HCID 81335 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Tert-butyl (piperidin-4-ylmethyl)carbamate | HCID 723429 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Nitrobenzene | HCID 7416 | — |
Reaction Steps
To a solution of 2,3-difluoronitrobenzene (5.0 g, 31 mmol) in EtOH (25 mL) were added tert-butyl piperidin-4-ylmethylcarbamate (8.1 g, 38 mmol), and N,N-diisopropylethylamine (6.6 mL, 38 mmol). The reaction was irradiated to 110° C. for 20 min by microwave. The crude reaction mixture was diluted with EtOAc, washed with 1 N HCl and brine, dried over MgSO4 and concentrated to yield nitrobenzene Int-2a (11.2 g, 99%) as yellow crystals. The crude product was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08623857B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-a7276f9a675a4ac396313baed90f7c1a |
| Source note | uspto-grants-2014_01 |