HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 117770182, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 117769717 | HCID 117769717 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 117770182 | HCID 117770182 | — |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A mixture of 5-bromo-4-hydroxy-1-isobutyl-2-oxo-1,2-dihydropyridine-3-carbonitrile obtained in Step B (6.6 g) and phosphorus oxychloride (0.126 mL) was heated at 120° C. for 24 hr, and cooled to room temperature. The reaction mixture was poured into water, and the pH was adjusted to 10 with potassium carbonate. The reaction mixture was extracted with ethyl acetate. The extract was washed with washed with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to give the title compound (4.60 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085578B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-c01e5c0298744a2bbe47cd187d10e0eb |
| Source note | uspto-grants-2015_07 |