Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 25143768 | HCID 25143768 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 25143769 | HCID 25143769 | — |
Reaction Steps
To a solution of potassium hydroxide (19 grams) in methanol (114 ml), 3-cyano-N,N-diethyl-5-methyl hexanamide (9.5 grams) was added followed by ammonia solution (38 ml) and Raney nickel (19 grams). Hydrogen pressure of 4.0 kg/cm2 was applied and the reaction mixture was stirred at 30° C. for 22 hours. The reaction mixture was filtered through a hyflow bed. The solvent was distilled off under reduced pressure at a temperature below 60° C. Water (200 ml) was added to the reaction mixture and pH adjusted to 2 with concentrated hydrochloric acid. The aqueous layer was extracted with dichloromethane. The pH of aqueous layer was adjusted to 8.0, with 50% sodium hydroxide. The aqueous layer was extracted with dichloromethane. The solvent was distilled off completely under atmospheric pressure to obtain the title compound as a residue.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08168828B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-c4230f41c26440ed893876a921bc3041 |
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| Source note | uspto-grants-2012_05 |
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