Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 54368073 | HCID 54368073 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54487707 | HCID 54487707 | 89% |
Reaction Steps
To an ice-cooled solution of (R)-2-amino-8-(4-butylpiperazin-1-yl)-1,2,3,4-tetrahydronaphthalene (100 mg, 0.35 mmol) and triethylamine (53 μL, 0.53 mmol) in methylene chloride (25 mL) was added dropwise acetyl chloride (25 μL, 0.35 mmol) in methylene chloride (10 mL). After the addition the reaction was allowed to stir at ambient temperature for 15 min and was then washed with water. The methylene chloride phase was dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified on a silica gel column using chloroform/ethanol saturated with NH3 (100:3) as the eluent. This gave, after crystalization from diethyl ether, 100 mg (89% yield) of the title compound as white crystals: mp 118-120° C.; [α]21D +25° (c 0.54, chloroform); EIMS (70 eV) m/z (relative intensity) 329 (41, M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06410530B1 |
|---|
| Source dataset | uspto-grants-2002_06 |
|---|
| ORD ID | ord-343f5a2644514f698fc4eedcfd2c69d3 |
|---|
| Source note | uspto-grants-2002_06 |
|---|