Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2-Bromotoluene | HCID 7236 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | HCID 23048980 | HCID 23048980 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23048938 | HCID 23048938 | 96.1% |
Reaction Steps
To a suspension of magnesium turnings (1.72 g, 0.071 mole) in anhydrous tetrahydrofuran (20 ml), 2-bromotoluene (12.1 g, 0.071 mole) in tetrahydrofuran (100 ml) was added dropwise under nitrogen. The reaction mixture was heated at reflux for 1 h after the initial exotherm had subsided before cyclopropyl-(N-methylpyrrol-2-yl)ketone (7.1 g, 0.047 mole) (J. Org. Chem., (1971), 36, 2897; J.Org.Chem. (1980), 45, 3172) in anhydrous tetrahydrofuran (100 ml) was introduced. After heating the reaction mixture at reflux for 2 h it was left overnight at room temperature. Saturated, aqueous ammonium chloride solution (100 ml) was added, and the mixture was extracted with diethyl ether (3×200 ml). The combined extracts were dried (MgSO4) and the solvents evaporated. The residue was flash chromatografied on silica gel eluting with n-heptane/tetrahydrofuran (19:1) providing the title compound as a solid (10.9 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04931450 |
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| Source dataset | uspto-grants-1990_06 |
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| ORD ID | ord-e794300c6be94363bc08d445e21d1074 |
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| Source note | uspto-grants-1990_06 |
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