HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178507473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 4-Amino-3-nitrobenzonitrile | HCID 595901 | — |
| Catalyst | Zinc bromide | HCID 10421208 | — |
| Product | HCID 178507473 | HCID 178507473 | 87% |
Reaction Steps
A mixture of 4-amino-3-nitrobenzonitrile (8-1) (163 mg, 1.0 mmol), NaN3 (1.5 mL of 2.0 M solution, 3.0 mmol) ZnBr2 (1.0 mL of 2.0 M solution, 2.0 mmol) was microwaved (Smith-Synthesizer) at 160° C. for 15 min with stirring. After this time, the reaction was completion according to LCMS. The reaction mixture was acidified to pH=2 with concentrated HCl. The precipitated product was collected by filtration and washed with water (2×3 mL). After drying, 179 mg (87%) of desired product were obtained as a yellow solid. Analytical LCMS: single peak, (214 nm), 1.909 min; 1H NMR (500 MHz, DMSO-d6): δ 8.70 (d, J=2.0 Hz, 1H), 8.02 (dd, J=8.9, 2.0 Hz, 1H), 7.92 (s, 2H), 7.21 (d, J=8.9 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07223738B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-d84606aff09f45de94ca327f2ab3d3c3 |
| Source note | uspto-grants-2007_05 |