Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Bromide | HCID 6332 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | 2,2,7,7-Tetramethylcycloheptan-1-one | HCID 13212145 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 13782560 | HCID 13782560 | 76.4% |
Reaction Steps
A mixed solution of ethyl bromide (33.30 g, 0.40 moles)/dried diethyl ether (40 ml) was dropped into a mixture of lithium (4.30 g, 0.62 moles)/dried diethyl ether (25 ml) in 2 hours while stirring at -30° C., followed by further adding dried diethyl ether (40 ml) and raising the temperature to 0° C. The mixture was subjected to separation by filtration. The resulting filtrate was dropped into a mixed solution of 2,2,7,7-tetramethylcycloheptanone (15.00 g, 0.09 moles)/dried diethyl ether (40 ml) in 30 minutes while stirring at 0° C. The mixture was stirred at 0° C. for 2 hours. The resulting reaction mixture was treated in the same manner as in Example 1 to obtain 13.50 g (yield 76.4%) of the captioned compound. This compound was a colorless transparent liquid having a woody, earthy and patchuli oil-like odor.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04631147 |
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| Source dataset | uspto-grants-1986_12 |
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| ORD ID | ord-3f1f0f61f78b404786c8092515adcb71 |
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| Source note | uspto-grants-1986_12 |
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