HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 7-Methoxy-4,5-dihydro-1H-benzo[D]azepin-2(3H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Acetamide, 2-chloro-N-(m-methoxyphenethyl)- | HCID 214755 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 7-Methoxy-4,5-dihydro-1H-benzo[D]azepin-2(3H)-one | HCID 13520689 | — |
Reaction Steps
N-chloroacetyl-N-(2-(3-methoxy-phenyl)-ethyl)-amine (3.1 g, 0.0136 mol) is dissolved in ethanol (270 ml) and water (1530 ml) and illuminated for 10 hours with a high pressure mercury lamp under a nitrogen atmosphere at 20°-25° C. The solution is evaporated down (to a volume of about 400 ml), mixed with sodium bicarbonate and extracted several times with ethyl acetate. The extracts are dried over magnesium sulphate, concentrated by evaporation and the residue is purified over a silica gel column with ethyl acetate as eluant.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04737495 |
| Source dataset | uspto-grants-1988_04 |
| ORD ID | ord-73cbc105f695482ba9d70bcca9f3fa40 |
| Source note | uspto-grants-1988_04 |