Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Lithium aluminum hydride | HCID 28112 | — |
| Reactant | Ethyl-4,4-difluorocyclohexane carboxylate | HCID 2779138 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (4,4-Difluorocyclohexyl)methanol | HCID 21184133 | 100.8% |
Reaction Steps
To a reaction mixture of 4,4-difluorocyclohexanecarboxylic acid ethyl ester (7.1 g, 37 mmol) in THF (50 mL) cooled to 0° C. was added dropwise 2.0 M lithium tetrahydroaluminate in THF (18.5 mL) over 10 min. The reaction mixture was stirred at 0° C. for 1 h. Water (5 mL) was added dropwise, followed by 1.0N NaOH (5 mL). The reaction mixture was filtered through Celite, THF was evaporated, and the resulting aqueous solution was diluted with brine (50 mL) and extracted with ethyl acetate (50 mL). The organic layer was collected, dried over anhydrous sodium sulfate, filtered, and concentrated to give the title compound as a clear oil (5.6 g) which was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07902220B2 |
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| Source dataset | uspto-grants-2011_03 |
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| ORD ID | ord-93d380babc0149ae8b4e5c23458b23d3 |
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| Source note | uspto-grants-2011_03 |
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