HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → HCID 10080884, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | 2,3,4,5-Tetrahydro-1H-benzo[c]azepine | HCID 10464472 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 10080884 | HCID 10080884 | — |
Reaction Steps
Acetic anhydride (20 ml) was added dropwise to formic acid (60 ml) at room temperature and after the mixture was stirred for 30 minutes, a solution of 2,3,4,5-tetrahydro 1H-2-benzazepine (10.71 g, 72.75 mmol) in ethyl acetate (5 ml) was added dropwise at room temperature. This mixture was stirred for 3 hours, after which it was diluted with ice-water and extracted with ethyl acetate. The extract was washed successively with water, aqueous solution of potassium carbonate (K2CO3), and saturated NaCl/H2O and dried over MgSO4. The solvent was then distilled off under reduced pressure and the residue was purified by silica gel column chromatography (eluent: ethyl acetate) to provide the title compound (11.35 g) as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06534496B1 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-3dc758339f814a6baef4e20b32934c81 |
| Source note | uspto-grants-2003_03 |