Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Reactant | HCID 53934625 | HCID 53934625 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54319692 | HCID 54319692 | 93.1% |
Reaction Steps
To an ice-cooled solution of (R)-2-amino-8-(4-propylpiperazin-1-yl)-1,2,3,4-tetrahydronaphthalene (85 mg, 0.31 mmol) and triethylamine (38 μL, 0.37 mmol) in methylene chloride (15 mL) was added acetyl chloride (23 μL, 0.31 mmol) in methylene chloride (5 mL) dropwise. 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 91 mg (93% yield) of the title compound as an oil which was crystallized from ethyl acetate/hexane. Yield: 61 mg (62%) as white crystals: mp 139-140° C.; [α]21D +26° (c 0.50, chloroform); EIMS (70 eV) m/z (relative intensity) 315 (78, M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06410530B1 |
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| Source dataset | uspto-grants-2002_06 |
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| ORD ID | ord-e29ddb1ba3854ba9b65c5aee8b0770f3 |
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| Source note | uspto-grants-2002_06 |
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