Nitrogen → 4-Methylenecyclohexylmethanol
反応式
[CH2:1]=[C:2]1[CH2:7][CH2:6][CH:5]([C:8](OCC)=[O:9])[CH2:4][CH2:3]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].N#N>CCOCC>[CH2:1]=[C:2]1[CH2:7][CH2:6][CH:5]([CH2:8][OH:9])[CH2:4][CH2:3]1参加物
5
実験手順
To a solution of ethyl 4-methylenecyclohexanecarboxylate (2 g, 11.89 mmol) in ether (40 mL) was added LAH (0.5 g, 13.17 mmol) portionwise under N2. The reaction mixture was refluxed for 1 h and was quenched by addition of 1 mL of EtOAc carefully and refluxed for 10 min. The reaction mixture was cooled down and added 3 mL of 1 N NaOH and stirred for 5 min, filtered off the solid and washed with ether. The filtration was washed with water, brine, dried (MgSO4), and removed the solvent to afford (4-methylenecyclohexyl)methanol.
後処理
- temperatureThe reaction mixture was refluxed for 1 h
- customwas quenched by addition of 1 mL of EtOAc carefully
- temperaturerefluxed for 10 min
- temperatureThe reaction mixture was cooled down
- additionadded 3 mL of 1 N NaOH
- filtrationfiltered off the solid
- washwashed with ether
- filtrationThe filtration
- washwas washed with water, brine
- dry with materialdried (MgSO4)
- customremoved the solvent
出典と根拠
- ORDレコード
- ord-a0061a12dab140388fdef6b0e824013a
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09326973B2
反応ノート
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