HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 178513220, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 178509458 | HCID 178509458 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178513220 | HCID 178513220 | 81.2% |
Reaction Steps
A stirred suspension of 2-((R)-indan-1-ylamino)-4H-benzo[d][1,3]oxazine-6-carbonitrile (example 117) (310 mg, 1.07 mmol), hydroxylamine hydrochloride (275 mg, 3.96 mmol), sodium carbonate (227 mg, 2.14 mmol) in ethanol (4 ml) and water (4 ml) was heated under reflux conditions for 17 h, water (10 ml) was added, the precipitate was collected by filtration, washed with water and hexane. The crude product was further purified by crystallization (diethyl ether/methanol 10:1) to yield the title compound as white solid (280 mg, 81%). MS (ISP): m/e=323.3 (M+H+); m.p. 206° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163740B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-0d7c6e87e6ea4724ab56dce391d79c88 |
| Source note | uspto-grants-2012_04 |