HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86725012, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium hydride | HCID 62714 | — |
| Reactant | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| Reactant | 7-fluoroquinoxalin-2(1H)-one | HCID 21727534 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86725012 | HCID 86725012 | 29.1% |
Reaction Steps
Lithium hydride (88 mg, 011 mmol) was added to a solution of 7-fluoroquinoxalin-2(1H)one (1.3 g, 7.8 mmol) in N,N-dimethylformamide (40 ml) under cooling on ice and the mixture was stirred at room temperature for 30 minutes. The mixture was cooled on ice and 2-(2-bromoethyl)-1,3-dioxolane (1.33 ml, 11 mmol) was added thereto. The obtained mixture was stirred at room temperature for 24 hours, water was then gradually added thereto and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The obtained crude product was purified by silica gel column chromatography (dichloromethane/methanol) to yield 0.6 g (29%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952010B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-4377bf453226494d9f1e44aa5a04d88a |
| Source note | uspto-grants-2015_02 |