HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 44548548, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium Sulfide | HCID 14804 | — |
| Reactant | 3-(Chloromethyl)pyridine hydrochloride | HCID 23394 | — |
| Reactant | HCID 86654213 | HCID 86654213 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 44548548 | HCID 44548548 | — |
Reaction Steps
494 mg (1.5 mmol) of 2-chloro-4-[4-(2-hydroxyethoxy)phenyl]-6-methoxypyridine-3,5-dicarbonitrile are initially charged in 5 ml of DMF, 140 mg (1.8 mmol) of sodium sulphide are added and the mixture is stirred at room temperature for 3 hours. 311 mg (2.25 mmol) of potassium carbonate and 307 mg (1.8 mmol) of 3-picolyl chloride hydrochloride are then added. The reaction mixture is stirred at 45° C. overnight and then purified by preparative HPLC (acetonitrile/water: 10:90→95:5, with 0.1% formic acid added). This gives 255 mg (40% of theory) of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08791146B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-00f9965224804a4c93abd2af6a47f460 |
| Source note | uspto-grants-2014_07 |