HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphoric Acid → HCID 22253352, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22596067 | HCID 22596067 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22253352 | HCID 22253352 | 92.2% |
Reaction Steps
A mixture of [4-(1-ethyl-propylamino)-6-methyl-2-(2,4,6-trimethyl-phenoxy)-pyridin-3-yl]-acetonitrile (800 mg, 2.27 mmol), 6 ml of 85% phosphoric acid and 2 ml of water was heated at reflux for 2 hours and cooled to room temperature. The reaction mixture was neutralized with 2N NaOH and extracted twice with chloroform. The chloroform layer was dried and concentrated to give a yellow solid. The solid was purified through silica gel column chromatography using hexane to 6% ethyl acetate in hexane as eluent to give 730 mg (92.2%) of a white solid. 1H NMR (CDCl3) δ 6.87(s,2H), 6.5(s,1H), 4.1(m,1H), 3.12(s,2H), 2.38(s,3H), 2.30(s,3H), 2.10(s,3H), 1.7–2.0(m,4H), 0.8(t,6H) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06992188B1 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-90e4c187ea754193b9decfa86417e038 |
| Source note | uspto-grants-2006_01 |