HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 21465922, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 21465915 | HCID 21465915 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21465922 | HCID 21465922 | 80.1% |
Reaction Steps
A solution of 5-(2-chlorophenyl)-1-isobutyl-2,3,4,5-tetrahydro-1H-[1]-benzazepin-2-one (2.7 g) and N-chlorosuccinimide (1.65 g) in dimethylformamide (10 ml) was stirred for 7 hours at 70° C. To the reaction mixture was added acetic acid ethyl ester (100 ml), which was washed with dilute hydrochloric acid and a saturated aqueous solution of sodium hydrogencarbonate, followed by drying over anhydrous sodium sulfate. The solvent was removed, and the residue was recrystallized from hexane/acetic acid ethyl ester to give 2.39 g of colorless crystals, m.p. 152°-154° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05698691 |
| Source dataset | uspto-grants-1997_12 |
| ORD ID | ord-341cd8842aea46f489ce8d2390744a41 |
| Source note | uspto-grants-1997_12 |