Ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetate → 2-(1,4-Dioxaspiro(4.5)decan-8-yl)ethan-1-ol
反応式
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([CH2:11][C:12](OCC)=[O:13])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>CCOCC>[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([CH2:11][CH2:12][OH:13])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1参加物
4
反応条件
- 温度
- 0 °C
実験手順
To a solution of ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetate from Step 1 (3.31 g, 14.5 mmol) in Et2O (80 mL) at 0° C. under N2 was added LiAlH4 (1M in THF, 13.66 mL, 13.66 mmol) in 15 min. The resulting mixture was stirred at 0° C. for another 20 min and quenched by addition of saturated aqueous NH4Cl solution, extracted with EtOAc, dried over Na2SO4. Filtration and evaporation to dryness gave the alcohol as white solid (2.76 g, 100%). LC/MC: 187.1 (MH)
後処理
- customquenched by addition of saturated aqueous NH4Cl solution
- extractionextracted with EtOAc
- dry with materialdried over Na2SO4
- filtrationFiltration and evaporation to dryness
出典と根拠
- ORDレコード
- ord-590d9d7fa83f48b487923e4be701d69d
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08912169B2
反応ノート
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