HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → 5-Acetyl-2-chloro-11-cyclopropyl-5,11-dihydro-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Dipyridodiazepinone deriv. 14 | HCID 463143 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Product | 5-Acetyl-2-chloro-11-cyclopropyl-5,11-dihydro-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one | HCID 19960030 | — |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
A mixture of 2-chloro-11-cyclopropyl-5,11-dihydro-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one and acetic anhydride with 4-dimethylaminopyridine was heated at 130° C. until a clear solution was obtained. The solvent was evaporated and the residue was chromatographed over silica gel with ethyl acetate/hexane to give 0.85 g of the title compound, which crystallized from isopropyl ether/ethyl acetate, m.p. 204°-206° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05620974 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-9c5e84728dd94713b44dce4cd3ac4ecc |
| Source note | uspto-grants-1997_04 |