HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 22392577, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus trichloride | HCID 24387 | — |
| Reactant | HCID 570528 | HCID 570528 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22392577 | HCID 22392577 | — |
Reaction Steps
A solution of phosphorous trichloride (7.2 mL, 82 mmol) in CH2Cl2 was added to a cooled 0° C. solution of 2-ethyl-4-nitro-pyridine 1-oxide (3 g, 17.8 mmol) in CH2Cl2. The reaction was stirred for 2 hours and then warmed up to rt. After 3 hours the mixture was poured into ice, made basic with 15% NaOH and extracted with EtOAc. The organic extracts were dried over Na2SO4 and concentrated to a yellow oil that solidified on standing (2.56 g, 95%). 1H NMR (400 MHz, CDCl3): δ 1.40 (t, J=7.6 Hz, 3 H), 3.14 (d, J=7.6 Hz, 2 H), 8.04 (d, J=5.6 Hz, 1 H), 8.06 (s, 1 H), 8.92 (d, J=5.6 Hz, 1 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07148226B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-9df77be80c03487e815f1bdd81544675 |
| Source note | uspto-grants-2006_12 |