Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 59179416 | HCID 59179416 | — |
| Catalyst | Cobalt | HCID 104730 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethanol, reaction products with ammonia, distn. residues | HCID 22020343 | — |
| Product | HCID 59179431 | HCID 59179431 | 35% |
Reaction Steps
3-(2,3-Dihydrofuro[3,2-c]pyridin-4-yl)propanenitrile (110 mg, 0.63 mmol) and Raney cobalt (200 mg) were suspended in 2M ammonia/ethanol solution (10 mL), and the suspension was stirred at room temperature for 13 hr under a hydrogen atmosphere. The catalyst was filtered through celite, and the filtrate was evaporated under reduced pressure. This was dissolved in dichloromethane (5 mL), triethylamine (173 μL, 1.24 mmol) and acetyl chloride (52.8 μL, 0.743 mmol) were added, and the mixture was stirred at room temperature for 20 min. The reaction solution was diluted with saturated aqueous sodium hydrogen carbonate solution and the mixture was extracted with dichloromethane. The extract was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (NH, methanol/ethyl acetate=0/100→10/90) to give the title compound (47 mg, yield 35%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08273761B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-1d71992ab24a477db76fb4ff5b4a07e5 |
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| Source note | uspto-grants-2012_09 |
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