HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 19607876, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 19607827 | HCID 19607827 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 19607876 | HCID 19607876 | 16.2% |
Reaction Steps
To 5-{N-methyl-N-[3-(3,4,5,6-tetrahydro-2H-pyran-2-yloxy)propyl]amino}-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.4 g) is added a mixture of acetyl chloride (0.5 ml) and acetic acid (5 ml) at room temperature, and the mixture is stirred overnight. The reaction solution is concentrated and the resulting residue is purified by silica gel column chromatography (eluent; dichloromethane:methanol=30:1), and further purified again by silica gel column chromatography (eluent; n-hexane:ethyl acetate=1:2) to give 5-[N-methyl-N-(3-acetyloxypropyl)amino]-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.06 g) as colorless amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05985869 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-12f793c8b8f74f1aac2befb19769480b |
| Source note | uspto-grants-1999_11 |