HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Nitroaniline → 1-Azido-4-nitrobenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Nitroaniline | HCID 7475 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | 1-Azido-4-nitrobenzene | HCID 137049 | 99.3% |
Reaction Steps
A solution of sodium nitrite (761 mg, 11 mmol) in water (5 mL) was added dropwise to a 0° C. solution of 4-nitroaniline (508 mg, 3.68 mmol) in trifluoroacetic acid (5 mL). After stirring for 10 minutes, a solution of sodium azide (1.55 g, 23.9 mmol) was added slowly. The resulting yellow suspension was stirred at room temperature for 5 hours. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate, filtered and concentrated. Purification by column chromatography gave 1-azido-4-nitrobenzene (600 mg, 99%). 1H NMR (400 MHz, CDCl3, δ): 8.16-8.19 (m, 2H), 7.05-7.09 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859591B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-ff08c3b6c4094b0a846b7c960e33125f |
| Source note | uspto-grants-2014_10 |