Ethyl-4,4-difluorocyclohexane carboxylate → (4,4-Difluorocyclohexyl)methanol
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1([F:19])[CH2:13][CH2:12][CH:11]([C:14](OCC)=[O:15])[CH2:10][CH2:9]1>C(OCC)C>[F:7][C:8]1([F:19])[CH2:13][CH2:12][CH:11]([CH2:14][OH:15])[CH2:10][CH2:9]1参加物
4
実験手順
To a suspension of lithium aluminum hydride (2.6 g, 69 mmol) in diethyl ether (160 mL,) was added slowly a solution of commercially available ethyl 4,4-difluorocyclohexanecarboxylate (Matrix, 11.0 g, 57 mmol) in diethyl ether (20 mL). The reaction mixture was refluxed for 4 hours, then cooled in an ice bath, quenched cautiously with sequential addition of water (2.6 mL.), 15% NaOH (2.6 mL) and water (7.8 mL) and extracted with ethyl acetate (3×100 mL). The mixture was filtered and concentrated to afford the title compound.
後処理
- temperatureThe reaction mixture was refluxed for 4 hours
- temperaturecooled in an ice bath
- customquenched cautiously with sequential addition of water (2.6 mL.), 15% NaOH (2.6 mL) and water (7.8 mL)
- extractionextracted with ethyl acetate (3×100 mL)
- filtrationThe mixture was filtered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-7b95e3d9547f4bf4b3e4863df1b23bd0
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07875639B2
反応ノート
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