HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 12986045, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 12986044 | HCID 12986044 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 12986045 | HCID 12986045 | 97.4% |
Reaction Steps
2-(3-Chlorophenoxy)-3-[3-(3-ethoxycarbonylpyridin-4-yl) -propoxy]pyridine (1.0 g, 2.4 mmol) obtained in Example 23 is dissolved in methanol (50 ml), and thereto is added a 1M aqueous sodium hydroxide solution (3.0 ml), and the mixture is heated under reflux for 2 hours. The methanol is evaporated under reduced pressure, and the pH value of the residue is adjusted to pH 4 with a 1M aqueous hydrochloric acid solution, and the mixture is extracted with chloroform/tetrahydrofuran (1:1) (50 ml×2), dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue is recrystallized from ethanol/diethyl ether to give the title compound (0.9 g) as colorless crystals, m.p. 142-144° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06765095B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-99d9dcc8c2c7462bb4ba761ec0556448 |
| Source note | uspto-grants-2004_07 |