HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 5-Phenyl-1,3-dihydro-2H-azepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 12502457 | HCID 12502457 | — |
| Solvent | 2-Methoxyethanol | HCID 8019 | — |
| Product | 5-Phenyl-1,3-dihydro-2H-azepin-2-one | HCID 57349874 | — |
Reaction Steps
The crude diethyl-(5-phenyl-3H-azepin-2-yl)-amine (12.47 g) is added to water (10.0 mL) and 2-methoxy-ethanol (40.0 mL) and the resulting mixture heated to reflux and stirred 4½ days. The volatiles are removed in vacuo and the residue diluted with dichloromethane and washed with 0.1N HCl (2×200 mL) and saturated aqueous NaHCO3 (2×200 mL). The organic layer is dried over Na2SO4 and concentrated in vacuo to give the crude title compound as a dark brown solid (9.63 g). This material is carried into the next reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188069B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-50907c63078445fbb22162bf191b09f2 |
| Source note | uspto-grants-2012_05 |