HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → 1-Chloro-4,5-difluoro-2-nitrobenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 4-Chloro-1,2-difluorobenzene | HCID 136519 | — |
| Product | 1-Chloro-4,5-difluoro-2-nitrobenzene | HCID 10130330 | 96.8% |
Reaction Steps
To a flask was added 4-chloro-1,2-difluorobenzene (8.97 g, 60.4 mmol), followed by adding 98% con. H2SO4 (16.1 mL, 302 mmol) and 65% con. HNO3 (5.0 mL, 66.4 mmol) at 0° C. The mixture was stirred at rt for 5 hours, then poured into ice water (500 mL). The resulted mixture was extracted with ethyl acetate (200 mL×3). The combined organic phase were washed with saturated aqueous NaHCO3 solution (200 mL×2) and brine (200 mL), dried over anhydrous Na2SO4, and concentrated in vacuo to give the title compound as yellow liquid (11.31 g, 96.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09326975B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-b51a08a62c8f412b80f03d07f4fab644 |
| Source note | uspto-grants-2016_05 |