Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Bromooctane | HCID 8140 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 53912347 | HCID 53912347 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57091148 | HCID 57091148 | 83% |
Reaction Steps
A mixture of (1R,2R,3R)-2-(benzyloxymethyl)-3-methoxy-4,4-dimethylcyclohexanol (7 mg) and sodium hydride (5 mg, 60% dispersion in oil) and n-octyl bromide (20 ml) in dry N,N-dimethylformamide (0.3 ml) was stirred for 2 hrs at room temperature. The mixture was cooled to 0° C., and the reaction was quenched by addition of water. The pH of the mixture was adjusted to pH 7 with 0.1N hydrochloric acid. The mixture was extracted with diethyl ether, and the combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. Purification of the residue by preparative thin layer chromatography (using n-hexane:ethyl acetate=10:1 as an eluent) gave benzyl [(1R,2R,6R)-2-methoxy-3,3-dimethyl-6-octyloxycyclohexyl]methyl ether (8 mg, 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05449785 |
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| Source dataset | uspto-grants-1995_09 |
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| ORD ID | ord-30f46a933f1240a7ae4e4d7907e97257 |
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| Source note | uspto-grants-1995_09 |
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