HuagongsheHuagongshe Chemistry Print Report · For research reference only
(4-Nitrophenyl)acetic acid → 2-(4-Nitrophenyl)acetohydrazide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (4-Nitrophenyl)acetic acid | HCID 4661 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(4-Nitrophenyl)acetohydrazide | HCID 287331 | — |
Reaction Steps
A solution of 4-nitrophenylacetic acid (2.81 mmol) in dry dichloromethane (10 ML) was treated with a 2N solution of oxalyl chloride (3.0 mL) and DMF (0.02 mL) via syringe, and the reaction stirred at ambient temperature for 1 h. The reaction was concentrated to dryness in vacuo and the crude product was dissolved in dry dichloro-methane (20 mL), treated with anhydrous hydrazine (11.1 mmol) via syringe, and stirred at ambient temperature for 18 h. The resulting suspension was filtered, solids rinsed with dichloromethane, dissolved in MeOH/CH2Cl2, filtered, and filtrate concentrated in vacuo giving the title compound as an orange solid. 1H NMR (DMSO-d6) δ 8.17 (2H, d, J=8.8 Hz,), 7.54 (2H, d, J=8.8 Hz), 3.54 (2H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030305B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-f7f7132b2e5348c8a623f92f4956e1f1 |
| Source note | uspto-grants-2011_10 |