HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pentanenitrile, 4,4-dimethyl-3-oxo- → HCID 66644209, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| Reactant | (Cyclopropylmethyl)hydrazine--hydrogen chloride (1/2) | HCID 43810474 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 66644209 | HCID 66644209 | 90% |
Reaction Steps
A mixture of Example 1B (13.5 g, 85 mmol) and 4,4-dimethyl-3-oxopentanenitrile (11.7 g, 93 mmol) in ethanol (100 mL) was heated at reflux for 6 hours. The mixture was cooled to room temperature, and concentrated under reduced pressure. The residue was diluted with ethyl acetate (20 mL). The resulting white precipitate was filtered, washed with ether, and dried to yield 17.5 g (90%) of title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.42-0.54 (m, 4 H), 1.16-1.27 (m, 1 H), 1.28 (s, 9 H), 4.38 (d, J=7.12 Hz, 2 H), 4.80 (br, 2 H), 5.53 (s, 1 H), 15.5 (br, 1 H); MS (DCI) m/z 194 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236822B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-f4f76006a7f142d0a4fc517c89a5c429 |
| Source note | uspto-grants-2012_08 |