HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 86650559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3,5-Dibromo-4-methoxybenzoyl chloride | HCID 33779630 | — |
| Reactant | 5-Chloro-3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine | HCID 70700745 | — |
| Solvent | Butyl ether | HCID 8909 | — |
| Product | HCID 86650559 | HCID 86650559 | 50% |
Reaction Steps
In a 50 ml flask equipped with a reflux apparatus, 5-chloro-3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine (890 mg, 5.22 mmol) was dissolved in butyl ether (20 ml), and 60% sodium hydride in mineral oil (250 mg, 6.26 mmol) was added and stirred at 1250 for 3.5 hours. The mixture was cooled to room temperature and 3,5-dibromo-4-methoxy-benzoyl chloride (2.06 g, 6.26 mmol) was added thereto and then stirred at 1250 for 24 hours. The mixture was cooled to room temperature and filtered and evaporated under reduced pressure. The residue was washed with methanol and dried under reduced pressure to obtain white solid (1.2 g, 50%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394792B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-f64b2efa4f3943b8a0e4a6f6d37c7a29 |
| Source note | uspto-grants-2013_03 |