HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 44608067, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3,5-Dibromo-4-methoxybenzoyl chloride | HCID 33779630 | — |
| Reactant | 7-Trifluoromethyl-2,3-dihydro-1H-pyrido[2,3-B][1,4]oxazine | HCID 66936691 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 44608067 | HCID 44608067 | 98% |
Reaction Steps
In a 5 ml flask, 7-trifluoromethyl-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine (27 mg, 0.23 mmol) and 3,5-dibromo-4-methoxy-benzoyl chloride (65 mg, 0.20 mmol) were dissolved in dichloromethane (0.6 ml), and then triethylamine (0.55 ml, 0.33 mmol) was added thereto dropwise at 0□. After stirring for 4 hours at room temperature, water was added and the mixture was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of methanol:dichloromethane=1:100. The fractions containing the product were collected and evaporated to obtain white solid (64 mg, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394792B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-35914bf01d7b47eb9e6e2d6f3352906a |
| Source note | uspto-grants-2013_03 |