Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dipropylamine | HCID 8902 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Potassium Bromide | HCID 253877 | — |
| Reactant | 3-Vinyl-cyclohex-2-enone | HCID 11768562 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 9920908 | HCID 9920908 | — |
Reaction Steps
3-Vinyl-cyclohex-2-enone (0.75 g, 6.1 mmol) (prepared according to Nasarow's method) was dissolved in acetonitril (1 mL) and dipropylamine (1.5 g, 16 mmol) was added followed by Cs2CO3 (50 mg). After stirring the mixture at rt for 3 h it was diluted with diethylether (100 mL), filtered and evaporated to dryness. The residue was destined in vacuo (175° C., 0.01 mm Hg) to give a slightly yellow oil which was converted to the hydrochloride salt. Recrystallization from isopropyl ether/isopropyl alcohol yielded: 1.2 g, 4.6 mmol (75%), mp 95-97° C. IR (KBr) 2962, 2613, 1667; 1H-NMR (CDCl3) δ 5.84 (d, 1H), 2.65 (m, 2H), 2.27-2.60 (m, 9H), 1.99 (m, 2H), 1.39-1.51 (m, 5H), 0.86 (t, 6H) ppm; 13C-NMR (CDCl3) δ 198.2, 163.5, 124.9, 54.2, 50.1, 35.7, 33.7, 28.4, 21.2, 18.5, 10.4 ppm; MS (EI) m/z 223 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | USRE042802E1 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-f34b449409154d72bb3cc9b36b18d5b8 |
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| Source note | uspto-grants-2011_10 |
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