HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22106074, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 22105947 | HCID 22105947 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22106074 | HCID 22106074 | 53.8% |
Reaction Steps
To a solution of N-[1-butyl-4-{3-(3-hydroxy-1-propynyl)phenyl}-1,2-dihydro-2-oxo-1,8-naphthyridin-3-yl]-N'-(2,6-diisopropylphenyl)urea (90 mg, 0.16 mmol) in methylene chloride (1.5 ml) were added carbon tetrabromide (81 mg, 0.245 mmol) and triphenylphosphine (51 mg, 0.196 mmol) under ice-cooling, and the mixture was stirred for 30 minutes. To the mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane: 1:5) to give the title compound (53 mg, 0.086 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05843957 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-288f94b6efdd4abda0421dc29acd1e09 |
| Source note | uspto-grants-1998_12 |