HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2-Difluoro-5-methoxy-6-nitrobenzo[d][1,3]dioxole → HCID 90413709, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2-Difluoro-5-methoxy-6-nitrobenzo[d][1,3]dioxole | HCID 90413978 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 90413709 | HCID 90413709 | 101.2% |
Reaction Steps
2,2-Difluoro-5-methoxy-6-nitrobenzo[d][1,3]dioxole (1.7 g, 7.3 mmol) was dissolved in ethyl acetate (50 mL) and treated with 5% palladium on carbon (200 mg) and hydrogen at 40-50 pounds per square inch (psi) on a shaker. After 90 min, the catalyst was removed by filtration, the solvent was removed by evaporation, and the product dried under vacuum to give the title compound as a brown solid (1.5 g, qt (quantitative)): 1H NMR (400 MHz, CDCl3) δ 6.63 (s, 1H), 6.50 (s, 1H), 3.82 (s, 3H), 3.76 (d, J=23.0 Hz, 2H); 19F NMR (376 MHz, CDCl3) δ −50.32 (s); EIMS m/z 203.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09149038B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-ade1e306c4f744f3adfe9e71a038c757 |
| Source note | uspto-grants-2015_10 |